CN112509805B - Method for optimizing magnetic property of cobalt-based magnetic thin film inductance material - Google Patents
Method for optimizing magnetic property of cobalt-based magnetic thin film inductance material Download PDFInfo
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- CN112509805B CN112509805B CN202011120297.7A CN202011120297A CN112509805B CN 112509805 B CN112509805 B CN 112509805B CN 202011120297 A CN202011120297 A CN 202011120297A CN 112509805 B CN112509805 B CN 112509805B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- 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
- H01F41/14—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 for applying magnetic films to substrates
- H01F41/18—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 for applying magnetic films to substrates by cathode sputtering
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- 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
- H01F41/14—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 for applying magnetic films to substrates
- H01F41/18—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 for applying magnetic films to substrates by cathode sputtering
- H01F41/183—Sputtering targets therefor
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- 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
- H01F41/14—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 for applying magnetic films to substrates
- H01F41/22—Heat treatment; Thermal decomposition; Chemical vapour deposition
Abstract
The invention discloses a method for optimizing magnetic property of a cobalt-based magnetic thin film inductance material, and belongs to the technical field of information storage and inductance. According to the technical scheme, the deposited sample is subjected to heat treatment at a proper temperature in a vacuum environment, so that the change of the interface structure of the sample is induced. The track structure at the ferromagnetic/nonmagnetic (Co-based soft magnetic material/MO) interface is adjusted through the Co-O track hybridization strength at the interface, a beneficial and proper Co-O track hybridization state is obtained, and the magnetic performance of the ferromagnetic thin film material is further adjusted and controlled.
Description
Technical Field
The invention belongs to the technical field of information storage and inductance, and particularly relates to a method for regulating and controlling a Co-based soft magnetic/non-magnetic interface structure through Co-O orbital hybridization strength adjustment so as to optimize the magnetic performance of a film.
Background
In recent years, the rapid development of electronic information technology, the arrival of the 5G era, not only provides great convenience for people in production and life, such as application of smart homes, unmanned vehicles, wearable devices and the like, but also enables receiving devices of information terminals to be greatly improved, and higher requirements are put forward on the performance, reliability, miniaturization, energy conservation and the like of advanced electronic elements such as magnetic sensors, inductors, transformers and the like. Therefore, it is required to improve the soft magnetic performance of the Co-based soft magnetic thin film, which is an important component of an inductor, a transformer, or the like.
Currently, permalloy, ferrite, amorphous metal magnetic materials, and the like are used as magnetic core materials in magnetic thin film inductors. Compared with ferromagnetic materials, Co-based amorphous soft magnetic materials, such as CoZrTa, have strong saturation magnetization and smaller coercive force, so that the eddy current loss of the inductance device in high-frequency application can be reduced. Due to the intrinsic advantages, the Co-based amorphous soft magnetic material gradually becomes a core functional material in advanced electronic components such as inductors, transformers and the like. In order to further suppress the eddy current loss generated during the practical application of the inductive component, CoZrTa and Non-magnetic interface (NMIL) (e.g. SiO)2，Al2O3，AlN，Ta2O5Etc.) to be applied to inductance components, the introduction function of the oxide is to block the adjacent magnetic layers and regulate the magnetostatic coupling function of the adjacent magnetic layers so as to reduce the eddy current loss. The control of sputtering parameters (sputtering pressure, sputtering rate, etc.) and the control of target components (Co) have been developed internationally91.5Zr4Ta4.5，Co82Zr8Ta10，Co90Zr5Ta5，Co78.5Zr9.5Ta12Etc.), sputtering period of multilayer film, etc. regulation and control method [ AIP Advances 8(2018)048002]. However, due to the multilayer film [ CoZrTa/MO]n has more periodicity, and the thickness of the magnetic layer is thicker and generally more than 50-200 nm, so that the regulation and control capability of the macroscopic process on the magnetic performance of the film is limited. Therefore, how to reduce the complexity and difficulty of preparation and seek a method for effectively and simply regulating and controlling the magnetic performance of the FM/MO thin film on the premise of not requiring a complex sputtering process, is one of the key problems for preparing high-performance magnetic thin film inductive materials and devices.
The interface electronic structure regulation is an effective method for changing the performance of the magnetic heterojunction, and opens up a new idea for the performance regulation of the Co-based amorphous soft magnetic material CoZrTa. Through annealing at a proper temperature, effective oxygen migration can be generated at the interface, so that the reconstruction of interface oxygen atoms is triggered, the more beneficial orbital hybridization degree of Co and O is obtained at the interface, and the magnetic performance of the ferromagnetic thin film is improved and optimized.
Disclosure of Invention
At present, the reported magnetic performance regulation and control means are all used for regulating the performance of a sputtered film through exploration of a complex magnetron sputtering process, the component proportion of a Co-based soft magnetic material and the like, the regulation and control means generally have great dependence on sputtering parameters and conditions, the process is complex, and certain sample preparation cost is increased. Aiming at the existing technical problems, the invention aims to provide a method for adjusting the track structure at the ferromagnetic/nonmagnetic (Co-based soft magnetic material/MO) interface through the Co-O track hybridization strength at the interface to obtain a beneficial and proper Co-O track hybridization state, further regulating and controlling the magnetic property of a ferromagnetic thin film material, and improving and optimizing the magnetic property of the ferromagnetic thin film, and the method has the advantages of simple process, convenient control, high efficiency, low cost and the like.
In order to achieve the purpose, the invention provides the following technical scheme:
a method for optimizing the magnetic performance of a cobalt-based magnetic thin film inductance material comprises the following steps:
s1, cleaning the surface of a Co-based soft magnetic material target;
s2, depositing the Co-based soft magnetic material and the Al on the substrate in sequence by utilizing a magnetron sputtering method2O3Forming a Co-based soft magnetic material/Al2O3Structure;
and S3, after the deposition is finished, carrying out heat treatment at a proper temperature on the film system obtained in the step S2 in a vacuum environment.
Preferably, the Co-based soft magnetic material includes CoZrTa, CoZrTaB.
Preferably, the substrate comprises a Si substrate with a thermally oxidized SiO2 layer, a Si substrate, a stress strained substrate.
Further, the cleaning process in step S1 includes: firstly, carrying out ultrasonic cleaning on the surface of the target material by using an organic chemical reagent, then carrying out ultrasonic cleaning by using deionized water, and finally drying by blowing nitrogen or drying in an oven.
Further, the organic chemical agent includes acetone or alcohol.
Further, the background vacuum degree of the magnetron sputtering chamber in the step S2 is 1 × 10-5～3×10-5Pa, the argon pressure during sputtering is 0.3-0.8 Pa.
Further, the bombardment time of the Co-based soft magnetic material target material subjected to magnetron sputtering in the step S2 is 2-5 minutes, and Al2O3The target material bombardment time is 6-8 minutes.
Further, the vacuum degree of the vacuum environment in step S3 is 1 × 10-5～5×10-5Pa, the temperature of the heat treatment is 200-500 ℃, and the heat preservation time is 5-30 minutes.
The invention carries out simple vacuum annealing treatment on the sample to induce the change of the interface structure of the sample. Through the interfaceThe Co-O orbital hybridization strength is used for adjusting the orbital structure at the ferromagnetic/nonmagnetic (Co-based soft magnetic material a/MO) interface, so that a beneficial and proper Co-O orbital hybridization state is obtained, and the magnetic property of the ferromagnetic thin film material is further adjusted and controlled. When the deposited sample is heated by the heat treatment described in step S3, the Co-based soft magnetic material/Al2O3The transition process of oxygen migration at the interface occurs, so that the orbital hybridization intensity of Co-O changes. The effect of carrying out heat treatment on the sample in different temperature ranges is that the intensity of orbital hybridization of Co-O at the interface can be regulated to a great extent, and a large window is provided for effectively regulating and controlling the magnetic property through the interface oxygen environment.
The technical scheme provided by the invention has the beneficial effects that at least:
the sample is subjected to a simple vacuum annealing treatment to induce the change of the interface structure. The track structure at the ferromagnetic/nonmagnetic (Co-based soft magnetic material/MO) interface is adjusted through the Co-O track hybridization strength at the interface, so that a beneficial and proper Co-O track hybridization state is obtained, the magnetic performance of the ferromagnetic thin film material is further adjusted, and the method has the advantages of simple process, convenience in control, high efficiency, low cost and the like. Specifically, the method comprises the following steps:
(1) the Co-O track hybridization method for regulating and controlling the magnetic property of the Co-based magnetic thin film inductance material, provided by the invention, is used for carrying out simple vacuum annealing treatment on a sample to induce the change of the interface structure of the sample, and basically does not depend on sputtering parameters and conditions;
(2) the method can realize the adjustment of the film interface structure only through simple temperature control, further realize the effective regulation and control of the magnetism of the Co-based soft magnetic material, does not need complex micro-processing technology and expensive micro-structural equipment, has the advantages of simple process, convenient control, high efficiency, low cost and the like, and is suitable for being applied to the future information storage and inductance technology.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 is a graph showing the variation of the interface magnetic dead layer thickness (a), coercive force (b), and saturation magnetization (c) of a sample with the heat treatment temperature;
FIG. 2 is a schematic view showing the change of oxygen distribution at the interface before and after heat treatment of a sample.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be described in further detail below.
The invention provides a method for optimizing the magnetic property of a cobalt-based magnetic thin film inductance material, which induces the change of an interface structure of a sample by carrying out simple vacuum annealing treatment on the sample. The track structure at the ferromagnetic/nonmagnetic (Co-based soft magnetic material/MO) interface is adjusted through the Co-O track hybridization strength at the interface, so that a beneficial and proper Co-O track hybridization state is obtained, and the magnetic property of the ferromagnetic thin film material is further adjusted and controlled.
[ example 1 ]
S1, cleaning the surface of a CoZrTa target, wherein the specific cleaning process is as follows:
(1) ultrasonic cleaning with acetone alcohol;
(2) then ultrasonically cleaning by using deionized water;
(3) and finally blowing by nitrogen.
S2, sequentially depositing CoZrTa and Al on the silicon substrate by utilizing a magnetron sputtering method2O3Form CoZrTa/Al2O3Structure; firstly bombarding the CoZrTa target for 2 min and 50 sec, and then carrying out Al2O3Bombarding for 7 min and 48 sec with target material and sputtering chamber with background vacuum degree of 1 x 10-5Pa, argon pressure is 0.3Pa during sputtering;
s3, after deposition is finished, carrying out vacuum heat treatment on the sample, wherein the process is as follows: vacuum degree of 1X 10-5Pa, the temperature of heat treatment is 250 ℃, and the holding time is 30 minutes.
[ example 2 ]
S1, cleaning the surface of a CoZrTa target material, wherein the specific cleaning process is as follows:
(1) ultrasonic cleaning with acetone alcohol;
(2) then ultrasonically cleaning the glass substrate by using deionized water;
(3) and finally drying by nitrogen.
S2, sequentially depositing CoZrTa and Al on the silicon substrate by utilizing a magnetron sputtering method2O3Form CoZrTa/Al2O3Structure; firstly bombarding the CoZrTa target for 2 min and 50 sec, and then carrying out Al2O3Bombarding for 7 min and 48 sec with target material and sputtering chamber with background vacuum degree of 1 x 10-5Pa, argon pressure is 0.3Pa during sputtering;
s3, after deposition is finished, carrying out vacuum heat treatment on the sample, wherein the process is as follows: vacuum degree of 1X 10-5Pa, the temperature of the heat treatment is 350 ℃, and the holding time is 30 minutes.
[ example 3 ]
S1, cleaning the surface of a CoZrTa target material, wherein the specific cleaning process is as follows:
(1) ultrasonic cleaning with acetone alcohol;
(2) then ultrasonically cleaning the glass substrate by using deionized water;
(3) and finally blowing by nitrogen.
S2, sequentially depositing CoZrTa and Al on the silicon substrate by utilizing a magnetron sputtering method2O3Form CoZrTa/Al2O3Structure; firstly bombarding the CoZrTa target for 2 min and 50 sec, and then carrying out Al2O3Bombarding for 7 min and 48 sec with target material and sputtering chamber with background vacuum degree of 1 x 10-5Pa, the argon pressure is 0.3Pa during sputtering;
s3, after deposition is finished, carrying out vacuum heat treatment on the sample, wherein the process is as follows: vacuum degree of 1X 10-5Pa, the temperature of heat treatment is 450 ℃, and the holding time is 30 minutes.
FIG. 1 is a graph showing the variation of the interface magnetic dead layer thickness (a), coercive force (b), and saturation magnetization (c) of a sample with the heat treatment temperature. Preparation Structure of sample CoZrTa (5nm)/Al2O3(3nm) and the preparation conditions are as follows: thermally oxidized Si on the substrate, wherein the air pressure is 2mTorr during argon ion sputtering, the CoZrTa target material is bombarded for 2 minutes and 50 seconds firstly, and then Al is carried out2O3Target materialBombarding for 7 min and 48 sec, and backing vacuum degree of sputtering chamber of 1X 10-5Pa, argon pressure is 0.3Pa during sputtering; the samples were then subjected to vacuum heat treatment in the following procedure: vacuum degree of 1X 10-5Pa, the temperature of heat treatment is 250-450 ℃, and the heat preservation time is 30 minutes; subsequently, VSM test (sample size 3 mm. times.3 mm) was carried out to obtain the magnetic properties of the sample, i.e., the interface magnetic dead layer thickness (a), coercive force (b), and saturation magnetization (c) as a function of the heat treatment temperature. As can be seen from the figure, the thickness and coercive force of the magnetic dead layer are reduced, and the saturation magnetization is increased, indicating that the magnetic performance is optimized.
FIG. 2 is a schematic view showing the change of oxygen distribution at the interface before and after heat treatment of a sample. Corresponding CoZrTa and Al in the samples before heat treatment2O3The oxygen distribution state of (a) in FIG. 2, the degree of the Co-O orbital hybridization changes after the vacuum heat treatment with the vacuum degree of 3X 10-5Pa, the heat treatment temperature of 250 ℃ -450 ℃ and the heat preservation time of 5-30 minutes, as shown in (b) in FIG. 2.
As can be seen from FIGS. 1 and 2, when the thermal treatment temperature parameters are changed, i.e., the interface oxygen environment is gradually changed, CoZrTa/Al2O3The oxidation state of each element in the CoZrTa layer in the film is obviously changed, the oxidation is changed from weak oxidation in a preparation state to proper oxidation after heat treatment, and a proper Co-O orbital hybridization state at an interface is promoted, which indicates that: the heat treatment at proper temperature can effectively adjust the orbital hybridization strength at the interface of the ferromagnetic/nonmagnetic oxide, further regulate and control the magnetic performance of the thin film material, and has the advantages of simple process, convenient control, high efficiency, low cost and the like.
[ example 4 ]
S1, cleaning the surface of a CoZrTaB target, wherein the specific cleaning process is as follows:
(1) ultrasonic cleaning with acetone alcohol;
(2) then ultrasonically cleaning by using deionized water;
(3) and finally blowing by nitrogen.
S2, sequentially depositing CoZrTaB and Al on the silicon substrate by utilizing a magnetron sputtering method2O3Form CoZrTaB/Al2O3Structure; firstly bombarding the CoZrTaB target for 3 min and 7 sec, and then carrying out Al2O3Bombarding for 7 min and 48 sec with target material and sputtering chamber with background vacuum degree of 1 x 10- 5Pa, the argon pressure is 0.3Pa during sputtering;
s3, after deposition is finished, carrying out vacuum heat treatment on the sample, wherein the process is as follows: vacuum degree of 1X 10-5Pa, the temperature of heat treatment is 250 ℃, and the holding time is 30 minutes.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and should not be taken as limiting the scope of the present invention, which is intended to cover any modifications, equivalents, improvements, etc. within the spirit and scope of the present invention.
Claims (4)
1. A method for optimizing magnetic performance of a cobalt-based magnetic thin film inductance material is characterized by comprising the following steps:
s1, cleaning the surface of a Co-based soft magnetic material target;
s2, depositing the Co-based soft magnetic material and the Al on the substrate in sequence by utilizing a magnetron sputtering method2O3Forming a Co-based soft magnetic material/Al2O3Structure;
s3, after the deposition is finished, carrying out heat treatment at a proper temperature on the film system obtained in the step S2 in a vacuum environment;
the Co-based soft magnetic material comprises CoZrTa and CoZrTaB;
the background vacuum degree of the magnetron sputtering chamber in the step S2 is 1 × 10-5～3×10-5Pa, the argon pressure is 0.3-0.8 Pa during sputtering;
the vacuum degree of the vacuum environment in step S3 is 1 × 10-5～5×10-5Pa, the temperature of the heat treatment is 200-500 ℃, and the heat preservation time is 5-30 minutes.
2. The method of optimizing the magnetic properties of a cobalt-based magnetic thin film inductor material of claim 1, wherein: the substrate comprises SiO with thermal oxidation2A Si substrate, a stress strain substrate.
3. The method of claim 1, wherein the cleaning process in step S1 comprises: firstly, carrying out ultrasonic cleaning on the surface of the target material by using an organic chemical reagent, then carrying out ultrasonic cleaning by using deionized water, and finally drying by blowing nitrogen or drying in an oven.
4. The method of optimizing the magnetic properties of a cobalt-based magnetic thin film inductor material of claim 1, wherein: bombarding the Co-based soft magnetic material target subjected to magnetron sputtering in the step S2 for 2-5 minutes, wherein Al is contained in the target2O3The target material bombardment time is 6-8 minutes.
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| JP2001298227A (en) * | 2001-02-14 | 2001-10-26 | Nec Corp | Ferrromagnetic tunnel junction element, magnetic sensor and magnetic memory system |
| CN1839429A (en) * | 2003-09-30 | 2006-09-27 | 富士通株式会社 | Perpendicular magnetic recording medium and magnetic storage device |
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| US7692901B2 (en) * | 2006-12-13 | 2010-04-06 | Tdk Corporation | Magnetoresistive effect thin-film magnetic head with anti-ferromagnetic layer for magnetic domain control |
| US20100209741A1 (en) * | 2007-07-26 | 2010-08-19 | Showa Denko K.K. | Perpendicular magnetic recording medium, process for production thereof, and magnetic recording/reproduction apparatus |
| CN101260514B (en) * | 2008-04-10 | 2011-08-10 | 兰州大学 | Method and device for preparing high-frequency soft magnetic thin film |
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