CN113421733B - Method for increasing perpendicular magnetic anisotropy of ferromagnetic thin film material - Google Patents
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- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F10/00—Thin magnetic films, e.g. of one-domain structure
- H01F10/08—Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers
- H01F10/10—Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers characterised by the composition
- H01F10/12—Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers characterised by the composition being metals or alloys
- H01F10/14—Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers characterised by the composition being metals or alloys containing iron or nickel
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- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
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Abstract
The invention relates to a method for increasing the vertical magnetic anisotropy of a ferromagnetic film material, which is characterized in that the vertical magnetic anisotropy of a Co film is obviously enhanced by a method of depositing a Ta/TiC/Co/Ta multilayer film structure on a Si substrate after surface polishing and argon ion bombardment treatment, and performing heat treatment and cooling after deposition.
Description
Technical Field
The invention relates to the technical field of high-density information storage and sensing, relates to a method for regulating and controlling the perpendicular magnetic anisotropy of a ferromagnetic thin film material serving as a key core material unit in the field, and particularly provides a method for increasing the perpendicular magnetic anisotropy of the ferromagnetic thin film material.
Background
Magnetic Random Access Memories (MRAMs) have various excellent characteristics such as high speed, high density, and low power consumption, and are considered to be ideal memories in electronic devices. The core material of an MRAM device is a magnetic multilayer film having perpendicular magnetic anisotropy, and the magnetic anisotropy determines the power consumption, memory density, stability, and the like of the device. Therefore, the adjustment of the magnetic anisotropy of the magnetic thin film has very important practical value for the application of the MRAM device.
At present, a part of research work is carried out internationally aiming at the regulation and control of the magnetic anisotropy of ferromagnetic thin film materials, and the method mainly focuses on regulating the magnetic anisotropy of the ferromagnetic thin film by methods such as oxide regulation, voltage application, pulsed laser irradiation, lattice strain and the like, and the regulation and control effects of the methods are very sensitive to process conditions such as annealing temperature, electric field intensity, strain amount and the like; moreover, the subsequent treatment of these methods may also have certain influence on the structure of the ferromagnetic thin film, such as causing inter-diffusion of atoms between layers, local breakdown, cracking of the thin film, etc., which is not favorable for industrial production and application to some extent. Therefore, how to effectively and simply regulate and control the magnetic anisotropy of the ferromagnetic thin film material is one of the key problems in the preparation of high-efficiency MARM devices.
Disclosure of Invention
Based on this, an object of the present invention is to provide a method for increasing perpendicular magnetic anisotropy of a ferromagnetic thin film material, which is simple, convenient to control, efficient, and low-cost, and can increase perpendicular magnetic anisotropy of a ferromagnetic thin film material, thereby facilitating improvement of power consumption, storage density, and stability of an electronic device.
The present invention provides in one aspect a method of increasing perpendicular magnetic anisotropy of a ferromagnetic thin film material, comprising the steps of: depositing a Ta/TiC/Co/Ta multilayer film on the Si substrate after surface polishing and argon ion bombardment treatment, and performing heat treatment after the deposition is finished.
In an embodiment of the present invention, the method for increasing perpendicular magnetic anisotropy of a ferromagnetic thin film material includes the following specific steps:
s1, performing surface polishing and argon ion bombardment treatment on the Si substrate, wherein the thickness of the Si substrate is 0.5-0.7 mm; the surface roughness after polishing is 0.5-1.5 nanometers; the argon ion bombardment current is 5-15 mA, and the bombardment time is 3-5 minutes;
s2, depositing Ta atoms, TiC atoms, Co atoms and Ta atoms on the Si substrate in sequence to form a multilayer film structure with a Ta buffer layer/TiC/Co/Ta protective layer by using a magnetron sputtering method in step S1, wherein the background vacuum degree of a sputtering chamber is 1 multiplied by 10-5～3×10-5Pa, the working pressure of argon is 0.3-0.6 Pa; the thickness of the Ta buffer layer obtained by deposition is
The thickness of the TiC layer is
The thickness of the Co layer is
The thickness of the Ta protective layer is
The atomic ratio of Ti to C in the TiC layer is 1.2: 1-1: 1.4;
s3, performing heat treatment on the multilayer film structure obtained in the step S2 in a vacuum environment with the vacuum degree of 1 × 10-5～3×10-5Pa, the heat treatment temperature is 300-500 ℃, and the heat preservation time is 30-120 minutes; finally, cool to room temperature.
The invention also provides a ferromagnetic thin film material obtained by the method for increasing the perpendicular magnetic anisotropy of the ferromagnetic thin film material.
The principle of the invention is as follows: the surface polishing and the argon ion bombardment of the surface of the Si substrate have the effects of greatly reducing the roughness of the surface of the substrate and reducing the oxide layer of the surface so as to ensure that the subsequently deposited film can generate good texture and interface quality. And depositing a Ta/TiC/Co/Ta multilayer film structure on the treated Si substrate, and performing heat treatment at 300-500 ℃ to enable the TiC layer and the Co layer to generate proper interface atomic fusion. On one hand, the (002) texture of the Co thin film is enhanced through the lattice epitaxy between Ti and Co; on the other hand, by utilizing proper hybridization between the 3d electron of the Co atom and the 2p electron of the C atom, the energy band splitting of the Co is adjusted to increase the energy difference of the perpendicular magnetization and the in-plane magnetization of the Co thin film, and finally the perpendicular magnetic anisotropy is remarkably increased.
The invention has the beneficial effects that: according to the invention, only a proper TiC buffer layer is introduced in the process of preparing the Co film by using the ferromagnetic film material, so that the vertical magnetic anisotropy of the Co film can be obviously enhanced. That is to say, the method for increasing the perpendicular magnetic anisotropy of the ferromagnetic thin film material does not need high-cost rare metals or expensive additional devices, so that the method has the advantages of simple preparation, convenient control, high efficiency, low cost and the like, is suitable for being applied to the future spintronics technology, and the ferromagnetic thin film material prepared by the method has high perpendicular magnetic anisotropy, and can improve the power consumption, storage density and stability of electronic devices applied by the ferromagnetic thin film material.
Further objects and advantages of the invention will be fully apparent from the ensuing description and drawings.
Drawings
FIG. 1 is a block flow diagram of the method of increasing perpendicular magnetic anisotropy of a ferromagnetic thin-film material according to the invention;
fig. 2 is a hysteresis loop of a ferromagnetic thin film obtained by the method for increasing perpendicular magnetic anisotropy of a ferromagnetic thin film material according to the first preferred embodiment of the present invention;
fig. 3 is a hysteresis loop of a ferromagnetic thin film obtained by the method for increasing perpendicular magnetic anisotropy of a ferromagnetic thin film material according to a second preferred embodiment of the present invention;
FIG. 4 is a graph of the magnetic anisotropy energy (K) of a ferromagnetic thin film prepared according to a second preferred embodiment of the present invention as a function of the TiC thickness (t);
fig. 5 is a hysteresis loop of a ferromagnetic thin film obtained by the method for increasing perpendicular magnetic anisotropy of a ferromagnetic thin film material according to a third preferred embodiment of the present invention.
Detailed Description
The following description is presented to disclose the invention so as to enable any person skilled in the art to practice the invention. The preferred embodiments in the following description are given by way of example only, and other obvious variations will occur to those skilled in the art. The basic principles of the invention, as defined in the following description, may be applied to other embodiments, variations, modifications, equivalents, and other technical solutions without departing from the spirit and scope of the invention.
It will be understood by those skilled in the art that in the present disclosure, the terms "vertical," "lateral," "up," "down," "front," "back," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like are used in the orientation or positional relationship indicated in the drawings for ease of description and simplicity of description, and do not indicate or imply that the referenced device or element must have a particular orientation, be constructed and operated in a particular orientation, and thus, the above terms should not be construed as limiting the present invention.
It is understood that the terms "a" and "an" should be interpreted as meaning that a number of one element or element is one in one embodiment, while a number of other elements is one in another embodiment, and the terms "a" and "an" should not be interpreted as limiting the number.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; may be mechanically connected, may be electrically connected or may be in communication with each other; either directly or indirectly through intervening media, either internally or in any other relationship. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
In the field of ferromagnetic thin film material preparation, the method of adjusting the magnetic anisotropy of the ferromagnetic thin film material by oxide adjustment, voltage application, pulsed laser irradiation, lattice strain and the like is mainly focused at present, the adjusting and controlling effect is very sensitive to the process conditions, and certain influence may be generated on the structure of the thin film, such as interdiffusion of interlayer atoms, local breakdown, thin film cracking and the like, which is not beneficial to industrial production and application to a certain extent. Based on the method, the preparation method of the ferromagnetic thin film material is simple, convenient to control, high in efficiency and low in cost, can increase the perpendicular magnetic anisotropy of the ferromagnetic thin film material, and is beneficial to improving the power consumption, storage density and stability of electronic devices.
Specifically, the ferromagnetic thin film material is prepared by depositing a Ta/TiC/Co/Ta multilayer film structure on a Si substrate after surface polishing and argon ion bombardment treatment, and performing heat treatment and cooling after deposition is finished. In the invention, the vertical magnetic anisotropy of the Co film can be obviously enhanced by introducing a proper TiC buffer layer in the process of preparing the Co film of the ferromagnetic film material.
The principle of the invention is as follows: the surface polishing and surface argon ion bombardment of the Si substrate have the following functions: the roughness of the surface of the substrate can be greatly reduced, and the oxide layer on the surface can be reduced, so that the subsequent deposited film can generate good texture and interface quality. And depositing a Ta/TiC/Co/Ta multilayer film structure on the treated Si substrate, and performing heat treatment at 300-500 ℃ to enable the TiC layer and the Co layer to generate proper interface atomic fusion. On one hand, the (002) texture of the Co thin film is enhanced through the lattice epitaxy between Ti and Co; on the other hand, by utilizing proper hybridization between the 3d electron of the Co atom and the 2p electron of the C atom, the energy band splitting of the Co is adjusted to increase the energy difference of the perpendicular magnetization and the in-plane magnetization of the Co thin film, and finally, the perpendicular magnetic anisotropy of the ferromagnetic thin film material is remarkably increased.
It can be understood that, the invention adopts the silicon substrate processed by surface polishing and argon ion bombardment, and utilizes the magnetron sputtering method to sequentially deposit Ta atoms, TiC atoms, Co atoms and Ta atoms on the processed silicon substrate to form a multilayer film structure with Ta/TiC/Co/Ta, thereby enhancing the vertical magnetic anisotropy of the ferromagnetic thin film material. The preparation method of the ferromagnetic thin film material has good regulation and control effect and is insensitive to process conditions, and the proper interface atom fusion can be generated between the TiC layer and the Co layer through the heat treatment step, so that the structural stability of the ferromagnetic thin film material is ensured, and the influence on the structure of the ferromagnetic thin film is avoided: such as causing inter-diffusion of atoms between layers, localized breakdown, film cracking, etc.
Specifically, as shown in fig. 1, specific steps of a method of increasing perpendicular magnetic anisotropy of a ferromagnetic thin film material according to the present invention are illustrated.
As shown in fig. 1, the preparation method of the ferromagnetic thin film material comprises the steps of:
s1, performing surface polishing and argon ion bombardment treatment on the Si substrate, wherein the thickness of the Si substrate is 0.5-0.7 mm; the surface roughness after polishing is 0.5-1.5 nm; the argon ion bombardment current is 5-15 mA, and the bombardment time is 3-5 minutes;
s2, depositing Ta atoms, TiC atoms, Co atoms and Ta atoms on the Si substrate in sequence to form a multilayer film structure with a Ta buffer layer/TiC/Co/Ta protective layer by using a magnetron sputtering method in step S1, wherein the background vacuum degree of a sputtering chamber is 1 multiplied by 10-5～3×10-5Pa, the working pressure of argon is 0.3-0.6 Pa; the thickness of the Ta buffer layer obtained by deposition is
The thickness of the TiC layer is
The thickness of the Co layer is
The thickness of the Ta protective layer is
The atomic ratio of Ti to C in the TiC layer is 1.2: 1-1: 1.4; s3, heat treating the multilayer film structure obtained in the step S2 under vacuum environment with the vacuum degree of 1 × 10-5～3×10-5Pa, the heat treatment temperature is 300-500 ℃, and the heat preservation time is 30-120 minutes; and finally, cooling to room temperature to obtain the ferromagnetic thin film material.
It is understood that the surface polishing and the argon ion bombardment treatment are performed on the silicon substrate in the step S1 because the roughness of the surface of the silicon substrate and the oxide layer all affect the texture and the interface between the silicon substrate and the Ta buffer film. In step S1, after the surface polishing and the argon ion bombardment are performed on the silicon substrate, the roughness of the surface of the silicon substrate and the oxide layer on the surface of the silicon substrate can be greatly reduced, so as to ensure that the subsequently deposited film can generate good texture and interface quality.
It is to be noted that, in the step S1, the surface polishing and the argon ion bombardment treatment are preferably performed on the silicon substrate in this order.
It is also worth mentioning that the thickness of the silicon substrate can also affect the vertical anisotropy of the ferromagnetic thin film material, and the excessive thickness of the silicon substrate can affect the surface roughness and is not beneficial to the formation of the thin film texture; the silicon substrate is too thin, which easily generates a large amount of crystal defects and is not beneficial to the orbital hybridization in the thin film. Therefore, when preparing the ferromagnetic thin film material, the thickness of the silicon substrate is required to be as follows: in the step S1, the thickness of the silicon substrate is 0.5-0.7 mm; the surface roughness of the polished silicon substrate is 0.5-1.5 nanometers, so that good texture and interface quality can be formed between the silicon substrate and the Ta buffer layer.
Further, in the step S1, the specific operating parameters for the argon ion bombardment treatment on the silicon substrate are as follows: the argon ion bombardment current is 5-15 mA, and the bombardment time is 3-5 minutes, so that an oxide layer on the surface of the silicon substrate can be removed, and the subsequent deposited film can generate good texture and interface quality.
Further, in step S2, depositing Ta atoms, TiC atoms, Co atoms, and Ta atoms in sequence on the silicon substrate after surface polishing and bombardment treatment by using a magnetron sputtering method includes the following specific operating parameters: background vacuum of sputtering chamber 1X 10-5～3×10-5Pa, the working pressure of argon is 0.3-0.6 Pa; the thickness of the Ta buffer layer obtained by deposition is
The thickness of the TiC layer is
The thickness of the Co layer is
The thickness of the Ta protective layer is
Ti in TiC layerAnd C in an atomic ratio of 1.2:1 to 1: 1.4.
Preferably, the atomic ratio of Ti to C in the TiC layer is 1:1, and should be selected to be 1:1 in consideration of the lattice epitaxy effect of Ti on Co and the orbital hybridization effect between C and Co atoms.
It is worth mentioning that in the step S3, the specific operating parameters for performing the heat treatment on the multilayer film structure with Ta/TiC/Co/Ta in the vacuum environment are as follows: the vacuum degree of the vacuum environment is 1 multiplied by 10-5～3×10-5Pa, the heat treatment temperature is 300-500 ℃, and the heat preservation time is 30-120 minutes.
It is understood that, in step S3, the degree of vacuum of 1 × 10 is adopted-5～3×10-5Pa, the heat treatment temperature is 300-500 ℃, and the heat preservation time is 30-120 minutes as follows: the TiC layer and the Co layer can generate proper interface atom fusion, the structural stability of the ferromagnetic thin film material is ensured, and the influence on the structure of the ferromagnetic thin film is avoided: such as causing inter-diffusion of atoms between layers, localized breakdown, film cracking, etc.
It should be understood that the method for preparing the ferromagnetic thin film material of the present invention is also a method for actually increasing the perpendicular magnetic anisotropy of the ferromagnetic thin film material.
The method for increasing perpendicular magnetic anisotropy of ferromagnetic thin film material of the present invention will be described in detail with reference to specific embodiments as follows:
as shown in fig. 2, a first preferred embodiment of the present invention is specifically illustrated. The preparation conditions of the ferromagnetic thin film material of this embodiment are as follows:
firstly, carrying out surface polishing and argon ion bombardment treatment on a Si substrate, wherein the thickness of the substrate is 0.5 mm, and the surface roughness after polishing is 0.5 nm; the argon ion bombardment current was 5mA, and the bombardment time was 3 minutes.
Then, Ta atoms (with a thickness of Ta) are sequentially deposited on the treated Si substrate by a magnetron sputtering method
) TiC atoms (thickness of
) Co atoms (thickness of
) And Ta atoms (thickness of
) Thereby preparing the Si substrate-
Multilayer film with background vacuum degree of 1 × 10 before sputtering deposition- 5Pa, argon pressure during sputtering is 0.3 Pa. The atomic ratio of Ti to C in the TiC layer was 1.2: 1.
After the deposition is finished, the mixture is subjected to heat treatment in a vacuum environment with the vacuum degree of 1 multiplied by 10-5Pa, 300 deg.C/30 min to promote the ability of the TiC and Co layers to produce proper interfacial atomic fusion.
Then, a hysteresis loop of the sample is measured by using a comprehensive physical test system at room temperature, and the magnetic field direction of the hysteresis loop is along the film surface direction or perpendicular to the film surface direction, so that the in-plane curve and the perpendicular curve in the graph 2 are obtained.
As shown in fig. 3, a second preferred embodiment of the present invention is specifically illustrated. The preparation conditions of the ferromagnetic thin film material of this embodiment are as follows:
firstly, carrying out surface polishing and argon ion bombardment treatment on a Si substrate, wherein the thickness of the substrate is 0.6 mm, and the surface roughness after polishing is 1 nanometer; the argon ion bombardment current was 10mA, and the bombardment time was 4 minutes.
Then, Ta atoms (with a thickness of
) TiC atoms (thickness of
) Co atoms (thickness of
) And Ta atoms (thickness of
) Thereby preparing the Si substrate-
Multilayer film with background vacuum degree of 2X 10 before sputter deposition-5Pa, argon pressure during sputtering is 0.4 Pa. The atomic ratio of Ti to C in the TiC layer is 1:1.
After the deposition is finished, the mixture is subjected to heat treatment in a vacuum environment with the vacuum degree of 2 multiplied by 10-5Pa, 400 ℃/60 minutes to promote the ability of the TiC and Co layers to produce proper interfacial atomic fusion.
Then, a hysteresis loop of the sample is measured by using a comprehensive physical test system at room temperature, and the magnetic field direction of the hysteresis loop is along the film surface direction or perpendicular to the film surface direction, so that the in-plane curve and the perpendicular curve in the graph of fig. 3 are obtained.
Taking the ferromagnetic thin film material of the second preferred embodiment as an example, through the thickness of the TiC layer, a graph of the influence of the thickness of TiC on the magnetic anisotropy energy (K) thereof can be obtained, as shown in fig. 4. As can be seen from FIG. 4, the interfacial magnetic anisotropy energy is from-1.41X 10 with increasing TiC thickness6erg/cm3Increased to 1.07 x 106erg/cm3Remarkably increased by 2.48 multiplied by 106erg/cm3This shows that the introduction of the TiC layer can effectively enhance the perpendicular magnetic anisotropy of the Co thin film.
As shown in fig. 5, a third preferred embodiment of the present invention is specifically illustrated. The preparation conditions of the ferromagnetic thin film material of this embodiment are as follows:
firstly, carrying out surface polishing and argon ion bombardment treatment on a Si substrate, wherein the thickness of the substrate is 0.7 mm, and the surface roughness after polishing is 1.5 nm; the argon ion bombardment current was 15mA, and the bombardment time was 5 minutes.
Then, Ta atoms (with a thickness of Ta) are sequentially deposited on the treated Si substrate by a magnetron sputtering method
) TiC atoms (thickness of
) Co atoms (thickness of
) And Ta atoms (thickness of
) Thereby preparing the Si substrate-
Multilayer film with background vacuum degree of 3 × 10 before sputtering deposition-5Pa, argon pressure during sputtering is 0.5 Pa. The atomic ratio of Ti to C in the TiC layer is 1: 1.4.
After the deposition is finished, the mixture is subjected to heat treatment in a vacuum environment with the vacuum degree of 3 multiplied by 10-5Pa, 500 ℃/120 min to promote the ability of the TiC and Co layers to produce proper interfacial atomic fusion.
Then, a hysteresis loop of the sample is measured by using a comprehensive physical test system at room temperature, and the magnetic field direction of the hysteresis loop is along the film surface direction or perpendicular to the film surface direction, so that the in-plane curve and the perpendicular curve in the graph of fig. 5 are obtained.
It can be understood from fig. 2 to 5 that, when the preparation conditions, particularly the thickness of the TiC layer, are changed, the easy magnetization direction of the ferromagnetic thin film is changed from the in-plane direction to the perpendicular film-plane direction, which indicates that: the TiC layer can effectively adjust the magnetic anisotropy of the Co film.
The technical features of the above embodiments can be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the above embodiments are not described, but should be considered as the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above examples only express preferred embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (2)
1. A method of increasing perpendicular magnetic anisotropy of a ferromagnetic thin film material, comprising the steps of:
s1, performing surface polishing and argon ion bombardment treatment on the Si substrate, wherein the thickness of the Si substrate is 0.5-0.7 mm; the surface roughness after polishing is 0.5-1.5 nm; the argon ion bombardment current is 5-15 mA, and the bombardment time is 3-5 minutes;
s2, depositing Ta atoms, TiC atoms, Co atoms and Ta atoms on the Si substrate in sequence to form a multilayer film structure with a Ta buffer layer/TiC/Co/Ta protective layer by using a magnetron sputtering method in step S1, wherein the background vacuum degree of a sputtering chamber is 1 multiplied by 10-5～3×10-5 Pa, the working pressure of argon is 0.3-0.6 Pa; the thickness of the deposited Ta buffer layer is 80-150A, the thickness of the TiC layer is 5-40A, the thickness of the Co layer is 5-30A, and the thickness of the Ta protective layer is 60-200A; the atomic ratio of Ti to C in the TiC layer is 1.2: 1-1: 1.4;
s3, performing heat treatment on the multilayer film structure obtained in the step S2 in a vacuum environment with the vacuum degree of 1 × 10-5～3×10-5Pa, the heat treatment temperature is 300-500 ℃, and the heat preservation time is 30-120 minutes; finally, cool to room temperature.
2. A ferromagnetic thin film material obtained by the method for increasing perpendicular magnetic anisotropy of a ferromagnetic thin film material according to claim 1.
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