CN210403770U - Ferromagnetic alloy Co-Fe-C thin film device - Google Patents
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Abstract
The ferromagnetic alloy Co-Fe-C thin film device consists of a first tantalum layer, an alloy layer, a second tantalum layer and a silicon substrate layer; the first tantalum layer, the alloy layer, the second tantalum layer and the silicon substrate layer are sequentially overlapped from top to bottom, wherein the thickness of the first tantalum layer is 5 nanometers, the thickness of the alloy layer is 20 nanometers, the thickness of the second tantalum layer is 5 nanometers, and the thickness of the silicon substrate layer is 0.2mm and 0.5 mm. The utility model discloses can realize having more excellent magnetostriction coefficient, energy attenuation coefficient and the heat stability than Co-Fe-B alloy simultaneously under specific carbon element content, all have the potentiality of using at magnetoelectric coupling device and spintronics device.
Description
Technical Field
The utility model relates to a ferromagnetic alloy thin film device who has high magnetostriction coefficient, low energy attenuation coefficient and high thermostability simultaneously has wide application's potentiality in the electronics field, belongs to electronics and material engineering field.
Background
In recent years, the search for ferromagnetic alloy materials with excellent properties has been a challenging issue. The development of novel magnetic devices requires that ferromagnetic materials have multiple excellent properties, and the development of research work in related structure and material fields is promoted. As early as 70 s of the last century, the traditional binary ferromagnetic alloy material NixCo1-x,NixFe1-xAnd CoxFe1-xDevelopment of magnetic devices has been expanding, but requires materials capable of industrial scale, isotropic, nanoscale flatness for thin film growth. Researches find that the growth of large-scale flat films is facilitated by doping a small amount of non-metallic elements into the back substrate of the binary ferromagnetic alloy material. Among them, the ferromagnetic nonmetal alloy Co-Fe-B film is a star material in the field of spintronics because of having perfect soft magnetism, extremely high spin polarizability, controllable magnetic anisotropy and extremely easy industrialized scale growth. However, the thermal stability of the properties of the Co-Fe-B alloy thin film is not high, and the damage to the properties of the alloy due to a high-temperature working environment exceeding 350 ℃ or thermal annealing during the preparation process is extremely significant, which is very unfavorable for the magnetic device requiring long-time working under current and voltage environments. In the past, researchers have realized the improvement of device thermal stability by replacing the materials of the buffer layer and the surface layer in the composite structure of Co-Fe-B/MgO. They do not consider replacing the alloy layer material to improve the thermal stability of the device.
Meanwhile, the ferromagnetic non-metal alloy Co-Fe-The magnetostrictive coefficient and the energy attenuation coefficient of the B film are not excellent. Typical values for the magnetostriction coefficient of Co-Fe-B films are 20 parts per million, which is an order of magnitude different than the superior systems (as measured by Hunter et al in annealed Co-Fe alloy films). The insufficient excellent magnetostriction coefficient limits the conversion efficiency between mechanical energy and magnetic energy of the film in the application of magnetoelectric coupling devices. By designing the structure of the Co-Fe-B alloy thin film device, the energy attenuation coefficient can be improved to 0.004, but the energy attenuation coefficient is improved to be equal to that of the magnetic oxide Y3Fe5O12The system is still very different. Thus, the efficiency and sensitivity of thin films for energy transfer in microwave devices is limited. It is noted that, in the existing alloy materials, the magnetostriction coefficient, the energy attenuation coefficient and the thermal stability may have a certain coefficient to be particularly excellent, but no material system can be simultaneously excellent.
Therefore, it is very urgent and necessary to find an alloy material which has more excellent properties than the thin film of Co-Fe-B alloy, especially three large coefficients and is excellent.
Disclosure of Invention
The present invention overcomes the above-mentioned shortcomings of the prior art and provides a ferromagnetic alloy Co-Fe-C thin film device.
The utility model discloses in ferromagnetic non-metallic alloy Co-Fe-C film system, look for the optimum composition that has high magnetostriction coefficient, low energy attenuation coefficient and high thermostability simultaneously and make the device on this basis.
The utility model provides a ferromagnetic alloy Co-Fe-C thin film device, which consists of a first tantalum layer as a surface layer, an alloy layer, a second tantalum layer as a buffer layer, a silicon oxide layer and a silicon substrate layer; the first tantalum layer, the alloy layer, the second tantalum layer, the silicon oxide layer and the silicon substrate layer are sequentially overlapped from top to bottom, wherein the thickness of the first tantalum layer is 5 nanometers, the thickness of the alloy layer is 20 nanometers, the thickness of the second tantalum layer is 5 nanometers, the silicon oxide layer is a natural oxide layer 2 nanometers, and the thickness of the silicon substrate layer is 0.2mm and 0.5 mm.
The ferromagnetic alloy Co-Fe-C deviceThe magnetostriction coefficient measurement is carried out by processing the material into 30 multiplied by 3 multiplied by 0.2mm3The energy attenuation coefficient measurement of a strip (length, width and thickness) is required to be processed into 6X 5X 0.5mm3A rectangular shape (length × width × thickness).
In the device, the silicon substrate layer is monocrystalline silicon which is oriented in [001], polished on a single surface, has the resistivity of 1-100 ohm multiplied by centimeter and is not subjected to any special treatment by natural oxidation on the surface.
The utility model discloses the ferromagnetic alloy Co-Fe-C film device who finds with optimum composition ratio, the utility model has the advantages that: the measured magnetostriction coefficient reaches 75 ppm, which is 3 times of that of widely used Co-Fe-B alloy, so that the conversion efficiency of mechanical energy and magnetic energy can be greatly improved in the application of magnetoelectric coupling devices; the measured energy attenuation coefficient reaches 0.002, which is half of that of Co-Fe-B alloy, so that the energy consumption can be more effectively saved and the sensitivity can be improved in the application of a spintronics device; the measured thermal stability reaches 500 ℃ which is far higher than 200-300 ℃ of the Co-Fe-B alloy, so that the device can work more stably under the conditions of high temperature, thermal annealing or large current.
Drawings
FIG. 1 is a side view of a thin film Co-Fe-C device made of ferromagnetic alloy having high magnetostriction coefficient, low energy attenuation coefficient and high thermal stability.
FIGS. 2-4 are high resolution electron micrographs of ferromagnetic alloy Co-Fe-C thin film devices at different carbon content.
Fig. 5 is a schematic diagram of an apparatus for performing magnetostriction coefficient testing on the device of the present invention, wherein the top view is shown on the left and the side view is shown on the right.
FIG. 6 shows the variation of the saturation magnetostriction coefficient of the device with the carbon content of the Co-Fe-C alloy layer when the device of the present invention is used for measuring the magnetostriction coefficient along the strip direction at room temperature.
Fig. 7 is a schematic diagram of an apparatus for performing an energy attenuation coefficient test on a device of the present invention.
FIG. 8 shows the variation of the energy attenuation coefficient of the device with the carbon content of the Co-Fe-C alloy layer when the device of the present invention is used for measuring the energy attenuation coefficient along the long direction at room temperature.
FIG. 9 shows the result of the energy attenuation coefficient test after different annealing temperature treatments when the Co-Fe-C alloy layer in the device contains 0%, 4.4% and 13.2% of carbon, respectively.
In fig. 1, 5 and 7, 1 is a first tantalum (Ta) layer, 2 is a ferromagnetic alloy (Co-Fe-C) layer, 3 is a second tantalum (Ta) layer, 4 is a naturally oxidized silicon oxide layer, 5 is a single-crystal silicon substrate layer, 6 is a clip for fixing a sample in a magnetostriction meter, 7 is an elongated device, 8 is a laser spot of which a sensor is focused at one end of the device, 9 is a coil electromagnet, 13 is a broadband microwave source in a broadband ferromagnetic resonance system, 14 is a coil electromagnet of a ferromagnetic resonance system, 15 is a coplanar waveguide, 16 is a rectangular device, and 17 is a lock-in amplifier for measuring an absorbed microwave signal.
Detailed Description
The utility model provides a ferromagnetic alloy Co-Fe-C film device with high magnetostriction coefficient, low energy attenuation coefficient and high thermal stability, the structure of which is shown in figure 1 and comprises a first tantalum layer 1, an alloy layer 2, a second tantalum layer 3, a natural oxidation layer 4 and a silicon substrate layer 5; the first tantalum layer 1, the alloy layer 2, the second tantalum layer 3, the natural oxidation layer 4 and the silicon substrate layer 5 are sequentially overlapped from top to bottom, wherein the thickness of the first tantalum layer 1 is 5 nanometers, the thickness of the alloy layer 2 is 20 nanometers, the thickness of the second tantalum layer 3 is 5 nanometers, the thickness of the natural oxidation layer 4 is 2 nanometers, and the thickness of the silicon substrate layer 5 is 0.2mm and 0.5 mm.
The utility model provides a ferromagnetic alloy Co-Fe-C film device who has high magnetostriction coefficient, low energy attenuation coefficient and high thermal stability simultaneously, its preparation process can adopt super high vacuum magnetron sputtering system, including following each step:
(1) purchase orientation [001]Two kinds of single crystal silicon wafers with single side polishing, resistivity of 1-100 ohm x cm, P type, thickness of 0.5 and 0.2mm, and processed into a silicon substrate layer 5, the size of the substrate layer 5 is long (along [100 ]]Direction) x width (in [010 ]]Direction) x thickness (Edge [001]]Direction) equal to 30X 3X 0.2mm3And 6X 5X 0.5mm3。
(2) Growing a second tantalum layer 3 serving as a buffer layer on the surface of the natural oxide layer 4 of the silicon substrate 5 by adopting a magnetron sputtering method, wherein the magnetron sputtering process parameters are as follows: vacuum pumping the backing to 10 deg.C using an ultra-high vacuum system at room temperature-6Below Pa, the film was grown by magnetron sputtering at a DC power of 30 watts for 150 seconds using a Ta target having a purity of 99.99%.
(3) And growing a 20-nanometer alloy layer 2 in situ on the second tantalum layer 3 by adopting a magnetron sputtering method, wherein the magnetron sputtering process parameters are as follows: vacuum pumping the backing to 10 deg.C using an ultra-high vacuum system at room temperature-6Pa or less, and Co of 99.99% purity0.5Fe0.5And C, maintaining DC 30W in Co0.5Fe0.5And (3) carrying out combined sputtering growth on the target by using 60-70 watts of radio frequency on the C target for about 20 minutes.
(4) And (3) growing a first tantalum layer 1 serving as a protective layer on the surface of the alloy layer 2 by adopting a magnetron sputtering method under the same magnetron sputtering condition as the second tantalum layer 3.
The utility model provides a ferromagnetic alloy Co-Fe-C film device with high magnetostriction coefficient, low energy attenuation coefficient and high thermal stability, which adopts the magnetron sputtering method to [001]]A buffer layer metal tantalum (Ta)3, a Co-Fe-C functional layer 2 and a surface layer metal tantalum (Ta)1 grow on a silicon substrate 5 which is tangential and single-sided polished and has a natural oxide layer 4. Other similar materials having similar surface roughness, e.g. Al2O3Quartz, etc., may also be used as the substrate. The carbon element content in the Co-Fe-C functional layer 2 is determined by the radio frequency power, in the embodiment, about 5% of carbon doping can be realized by applying 60-70 watts, and the carbon doping can be automatically adjusted according to the specific conditions of equipment. The utility model discloses utilize the magnetostriction measuring apparatu (fig. 5) and the broadband ferromagnetic resonance (FMR) system (fig. 7) of developing by oneself to carry out the measurement of magnetostriction coefficient and energy loss coefficient. In addition, the thermal stability of the alloy film is that the device is placed in a sealed tube furnace, and annealing is carried out at the temperature rise and temperature drop speed of 5 ℃ per minute and the high temperature of 100-500 ℃ under the high-purity argon protection environmentAfter one hour, the sample was cooled to room temperature and the energy attenuation coefficient was measured again.
According to the utility model discloses, the size of silicon substrate layer 5: is long (along [100 ]]Direction) x width (in [010 ]]Direction) x thickness (in [001]]Direction) 30X 3X 0.2mm3The method is suitable for measuring the magnetostriction coefficient; is long (along [100 ]]Direction) x width (in [010 ]]Direction) x thickness (in [001]]Direction) 6X 5X 0.5mm3Measurement of the energy attenuation coefficient; can be reasonably changed according to practical requirements. According to the utility model discloses, natural oxidation layer 4 can thicken to 2 ~ 20 nanometers according to actual need. According to the present invention, the thickness of the Co-Fe-C alloy layer 2 can be between 10 to 50 nm, preferably 20 nm. According to the utility model discloses, metal tantalum (Ta) that thickness can be in 2 ~ 40 nanometer within range is grown under the alloy-layer and on to 5 nanometers is preferred, as buffer layer 3, is the adhesion force that increases the alloy-layer on the substrate, as superficial layer 1, is to prevent wherein magnetic element Co, Fe from being oxidized.
The following introduces the utility model discloses an implementation:
firstly, a ferromagnetic alloy Co-Fe-C thin film device with high magnetostriction coefficient, low energy attenuation coefficient and high thermal stability is prepared.
Purchase orientation [001]A single-side polished single crystal silicon substrate, the substrate being processed to a length dimension (along [100 ]]Direction) x width (in [010 ]]Direction) x thickness (in [001]]Direction) equal to 30X 3X 0.2mm3And 6X 5X 0.5mm3Two kinds of substrates. Growing a buffer layer metal tantalum (Ta)3 on a natural oxide layer 4 of a silicon substrate by using an ultrahigh vacuum magnetron sputtering method, wherein the magnetron sputtering method comprises the following process parameters: using an ultra-high vacuum system at room temperature to vacuumize the back bottom to 10-6Pa, using Ta target material with purity of 99.99%, DC 30 watt to proceed magnetron sputtering growth for 150 seconds, thickness 5 nanometer. Then, the same ultrahigh vacuum magnetron sputtering device is used to deposit the catalyst on the Co0.5Fe0.5And C, sputtering and growing an alloy layer Co-Fe-C2 on the target material for about 20 minutes by using direct current of 30 watts and radio frequency of 60-70 watts respectively, wherein the thickness is 20 nanometers. Finally, the surface layer metal tantalum (Ta) is grown by 15 nanometers by the same method as the buffer layer metal tantalum (Ta), and the structure of the surface layer metal tantalum (Ta) is shown in figure 1Shown in the figure.
Fig. 2 to 4 are results of structural analysis of cross sections of devices containing different amounts of carbon element using a high-resolution electron microscope. When the device does not contain carbon element, the diffraction pattern of the alloy layer 2 is a lattice, indicating that the alloy layer is a crystalline thin film (fig. 2). When the device contains 13.2% of carbon, the diffraction pattern of the alloy layer 2 is a flare, indicating that the alloy layer is an amorphous film (fig. 4). While the diffraction pattern of alloy layer 2 is some circles when the device contains 4.4% carbon, indicating that the alloy layer is an intermediate film (fig. 3).
Next, the magnetostriction coefficient, the energy attenuation coefficient, and the thermal stability of the above devices were measured.
As shown in fig. 5, the dimensions will be 30 × 3 × 0.2mm3The device 7 is placed in a magnetostrictive gauge with one end of the device 7 fixed by a clamp 6 and the free end of the device 7 placed in the centre of a coil electromagnet 9. The device 7 is saturated and magnetized by a magnet with the magnetic field intensity of 5000 oersted along the strip direction, then the magnetic field is removed, the intensity of an alternating current magnetic field is slowly increased along the short strip direction, the change of the light reflection position of the free end is monitored by a laser spot 8 focused by a sensor, and the magnetostriction coefficient of the device 7 can be obtained through conversion of the measured displacement change. As shown in fig. 6, the magnetostriction coefficient of the device 7 is shown when the alloy layer 2 contains a different amount of carbon element. According to the result of the high resolution electron microscope analysis, the different amount of carbon elements can be divided into 3 regions, a crystalline thin film region 10, an amorphous thin film region 12 and an intermediate thin film region 11. The coefficient is optimum for an intermediate film having a content of about 5%.
As shown in fig. 7, the dimensions will be 6 × 5 × 0.5mm3The device 16 is placed on a coplanar waveguide 15 in a face-down manner, placed in the center of a coil electromagnet 14 of a broadband ferromagnetic resonance system, and provided with a direct current magnetic field applied along the short side length to be gradually reduced from 3000 oersted to 0, and a microwave signal generated by a broadband microwave source 13 flows through the coplanar waveguide 15 and is received by a lock-in amplifier 17. Monitoring the absorption of microwaves flowing through coplanar waveguide 15 at different frequencies requires measuring the absorption of microwaves at least 6 different frequencies. Absorber for sorting microwaves with different frequenciesThe peak width is narrowed and linear fitting is performed to obtain the energy attenuation coefficient of the device 16. As shown in fig. 8, the energy attenuation coefficient of the device 16 is shown when the alloy layer 2 contains carbon elements in different amounts. The coefficient is optimum for an intermediate film having a content of about 5%.
Mixing the above 30X 3X 0.2mm3And 6X 5X 0.5mm3The devices 7 and 16 are annealed for one hour at a high temperature of 100-500 ℃ under a high-purity argon protective environment at a temperature rise and temperature reduction speed of 5 ℃ per minute, cooled to room temperature, and then the energy attenuation coefficient measurement is continued, so that the rules at different annealing temperatures can be obtained. When different amounts of carbon elements are contained in the alloy layer 2, the difference in thermal stability can be found by comparing the law that the energy attenuation coefficient changes with the annealing temperature. As shown in FIG. 9, the thermal stability of the intermediate thin film having a carbon content of about 5% was the most preferable.
In conclusion, the intermediate Co-Fe-C alloy thin film device with about 5% of carbon element has better magnetostriction coefficient, energy attenuation coefficient and thermal stability than the Co-Fe-B alloy thin film, and has great significance for application.
The reason why the Co-Fe-C alloy film device prepared by the utility model has the best performance when the alloy layer 2 contains about 5 percent of carbon element is as follows:
the nanostructure of the alloy material has great influence on the mechanical response of the material under the action of an electric field or a magnetic field, and shows that the feedback of the mechanical response is particularly obvious when various structures are mixed in the material. This is because the interface energy triggered by the structure phase interface can improve the mechanical response coefficient of the material itself, and in the Co-Fe-C system, 5% doping is the maximum doping amount for improving the interface energy. The energy attenuation coefficient of the alloy material is related to the number of free electrons near the Fermi surface of the material, and the 5% doping is calculated to be the doping amount with the minimum number of free electrons near the Fermi surface of the material. While higher thermal stability is associated with a lower thermal relaxation coefficient of the material itself. The optimal values of the three properties can be realized in the alloy film with the same composition, and the alloy film has great significance in the application of magnetoelectric coupling devices and spintronics devices. The embodiments described in this specification are merely illustrative of implementations of the inventive concepts, and the scope of the invention should not be considered limited to the specific forms set forth in the embodiments, but rather the scope of the invention is intended to include equivalent technical means as would be understood by those skilled in the art from the inventive concepts.
Claims (1)
1. Ferromagnetic alloy Co-Fe-C thin film device, characterized in that: the buffer layer is composed of a first tantalum layer used as a surface layer, an alloy layer, a second tantalum layer used as a buffer layer, a natural oxidation layer and a silicon substrate layer; the first tantalum layer, the alloy layer, the second tantalum layer, the natural oxide layer and the silicon substrate layer are sequentially overlapped from top to bottom, wherein the thickness of the first tantalum layer is 5 nanometers, the thickness of the alloy layer is 20 nanometers, the thickness of the second tantalum layer is 5 nanometers, and the thickness of the silicon substrate layer is 0.2mm and 0.5 mm.
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