CN115094380B - FeCoCr magnetic material and preparation method and application thereof - Google Patents

FeCoCr magnetic material and preparation method and application thereof Download PDF

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CN115094380B
CN115094380B CN202210623362.0A CN202210623362A CN115094380B CN 115094380 B CN115094380 B CN 115094380B CN 202210623362 A CN202210623362 A CN 202210623362A CN 115094380 B CN115094380 B CN 115094380B
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fecocr
magnetic
layer
protective layer
hfo
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CN115094380A (en
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于广华
艾文祥
徐秀兰
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Shandong Maige Zhixin Electromechanical Technology Co ltd
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Shandong Maige Zhixin Electromechanical Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14Metallic material, boron or silicon
    • C23C14/16Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
    • C23C14/165Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08Oxides
    • C23C14/083Oxides of refractory metals or yttrium
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34Sputtering
    • C23C14/35Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • C23C14/352Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/58After-treatment
    • C23C14/5806Thermal treatment
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01DMEASURING NOT SPECIALLY ADAPTED FOR A SPECIFIC VARIABLE; ARRANGEMENTS FOR MEASURING TWO OR MORE VARIABLES NOT COVERED IN A SINGLE OTHER SUBCLASS; TARIFF METERING APPARATUS; MEASURING OR TESTING NOT OTHERWISE PROVIDED FOR
    • G01D5/00Mechanical means for transferring the output of a sensing member; Means for converting the output of a sensing member to another variable where the form or nature of the sensing member does not constrain the means for converting; Transducers not specially adapted for a specific variable
    • G01D5/12Mechanical means for transferring the output of a sensing member; Means for converting the output of a sensing member to another variable where the form or nature of the sensing member does not constrain the means for converting; Transducers not specially adapted for a specific variable using electric or magnetic means
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F10/00Thin magnetic films, e.g. of one-domain structure
    • H01F10/08Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers
    • H01F10/10Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers characterised by the composition
    • H01F10/12Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers characterised by the composition being metals or alloys
    • H01F10/14Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers characterised by the composition being metals or alloys containing iron or nickel
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F10/00Thin magnetic films, e.g. of one-domain structure
    • H01F10/08Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers
    • H01F10/10Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers characterised by the composition
    • H01F10/12Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers characterised by the composition being metals or alloys
    • H01F10/16Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers characterised by the composition being metals or alloys containing cobalt

Abstract

The invention discloses a FeCoCr magnetic material, a preparation method and application thereof. The FeCoCr magnetic material is sequentially provided with a Si substrate layer, a protective layer, a FeCoCr magnetic layer and a protective layer, wherein the protective layer is made of HfO 2 The thickness of each protective layer is 3nm-10nm, and the thickness of the FeCoCr magnetic layer is 100nm-300nm. The FeCoCr magnetic material provided by the invention can effectively prevent elements in the basal layer and the protective layer from diffusing into the FeCoCr magnetic layer, further has better magnetic performance, and has easy control of the preparation process and wide application prospect.

Description

FeCoCr magnetic material and preparation method and application thereof
Technical Field
The invention belongs to the technical field of magnetic materials, and relates to a FeCoCr magnetic material, a preparation method and application thereof.
Background
In the electric spindle system of the high-grade numerical control machine tool, the electric spindle system has high requirements on control precision, one of the more common schemes is to use a gear type magnetic encoder, and the magnetic encoder has the advantages of high precision and strong pollution resistance, but is only suitable for low-speed application, and has the problems of high noise, insufficient corresponding frequency and the like when being used under high-speed conditions. Thus, more and more advanced manufacturing facilities abroad are beginning to use magnetic coders of the type that magnetic coders write to magnetic poles, which are high precision magnetic coders. The high-precision magnetic encoder has various excellent characteristics of vibration resistance, high speed resistance, corrosion resistance, pollution resistance, low cost, simple structure and the like, and is further applied more and more in recent years. Wherein the core device constituting the magnetic encoder is a magnetic code wheel material having excellent magnetic properties. And, the comprehensive performance of the magnetic code wheel material and the like have important influence on the accuracy of the magnetic encoder and the stability control of the recorded magnetic signals. Therefore, the preparation of high-quality magnetic code wheel materials has great significance for the application of magnetic coding devices.
At present, the common magnetic code disc material is mainly ferrite blocks or FeCoCr alloy. In order to improve the signal writing density and signal quality, a technology for developing a Co-P, co-Ni-P film has been proposed, and a higher magnetic signal writing density can be obtained. However, the Co-P, co-Ni-P film is prepared by a chemical method and is not friendly to the environment. In addition, many other magnetic thin film materials have been proposed by researchers for high density data storage, such as: fePt, smCo, etc. However, the coercive force of the FePt and SmCo films is too high, so that the magnetic signal writing is not easy to perform well, and the films also have higher magnetic coupling effect, so that recording noise is increased.
In recent years, a technology for developing FeCoCr magnetic thin film materials has been proposed by researchers, and research into the regulation of magnetic properties thereof has been conducted. The FeCoCr magnetic film material is of a structure of Si substrate/FeCoCr/Ta, wherein Ta is a protective layer. However, it has been found that during the preparation of the thin film material, ta diffuses into FeCoCr due to the operation requiring high temperature annealing, which results in deterioration of magnetic properties, and Si in the underlayer diffuses into FeCoCr, which affects the material properties.
Therefore, how to obtain the FeCoCr magnetic film material which is convenient and environment-friendly in preparation method, low in cost and high in performance has very important research significance.
Disclosure of Invention
The invention solves the technical problem that in the FeCoCr magnetic thin film material structure in the prior art, ta is generally used as a protective layer, and the Ta protective layer on the top layer and the Si substrate layer on the bottom layer are both diffused into the FeCoCr layer in the middle, so that the magnetic performance of the material is seriously affected.
In order to solve the technical problems, the invention provides the following technical scheme:
in one aspect, the present invention provides a FeCoCr magnetic material comprising, in order, a Si base layer, a protective layer, a FeCoCr magnetic layer, and a protective layerThe protective layer is made of HfO 2 The thickness of each protective layer is 3nm-10nm, and the thickness of the FeCoCr magnetic layer is 100nm-300nm.
The FeCoCr magnetic material provided by the invention adopts HfO 2 The layer is used as a protective layer and Si substrate/HfO is adopted 2 /FeCoCr/HfO 2 In this type of structure, hfO is provided on both sides of the FeCoCr magnetic layer 2 As a protective layer, the defect that Ta element diffuses into a magnetic layer when Ta is adopted as the protective layer in the prior art can be overcome, and therefore the FeCoCr magnetic material is guaranteed to have good magnetic performance.
In particular, compared with the magnetic material using Ta as a protective layer in the prior art, the residual magnetism of the FeCoCr magnetic material provided by the invention is improved by about one time.
In some embodiments, the FeCoCr magnetic material has a structure of Si base layer/HfO 2 Protective layer/FeCoCr magnetic layer/HfO 2 And (3) a protective layer.
In some preferred embodiments, the FeCoCr magnetic material provided by the invention has the following structure: si substrate/HfO 2 (3nm~10nm)/FeCoCr(100nm~300nm)/HfO 2 (3nm~10nm)。
In some embodiments, each of the protective layers has a thickness of 5nm to 8nm and the FeCoCr magnetic layer has a thickness of 150nm to 280nm.
In some embodiments, in the FeCoCr magnetic layer, the Fe: co: the weight percentage of Cr is 40-50:25-30:20-30.
In some preferred embodiments, in the FeCoCr magnetic layer, the Fe: co: the weight percentage of Cr is 45:30:25.
In one aspect, the invention also provides a preparation method of the FeCoCr magnetic material, which comprises the following steps:
step S1, depositing the protective layer on the Si substrate layer by using a magnetron sputtering device and utilizing a magnetron sputtering method to obtain a first intermediate material;
s2, depositing the FeCoCr magnetic layer on the first intermediate material by utilizing a magnetron sputtering method to obtain a second intermediate material;
step S3, depositing the protective layer on the second intermediate material by utilizing a magnetron sputtering method to obtain the third intermediate layer;
and S4, carrying out vacuum annealing treatment on the third intermediate layer to obtain the FeCoCr magnetic material.
The preparation method of the FeCoCr magnetic material provided by the invention has the advantages of simple preparation process, easiness in control, high efficiency and low cost.
In some preferred embodiments, the reaction conditions of the magnetron sputtering method in the step S1 to the step S3 include: the pressure is 0.2 Pa-0.7 Pa, and the vacuum degree of the sputtering chamber is 1 multiplied by 10 -5 Pa~4×10 -5 Pa。
In some preferred embodiments, the deposition time in step S1 is 60S to 180S.
In some preferred embodiments, the deposition time in step S2 is 5min to 15min.
In some preferred embodiments, the deposition time in step S3 is 60S to 180S.
10. In some preferred embodiments, the reaction conditions for performing vacuum annealing in step S4 include: the annealing temperature is 550-700 ℃, the annealing time is 30-60 min, and the vacuum degree is 2X 10 -5 Pa~6×10 -5 Pa。
In one aspect, the invention further provides the FeCoCr magnetic material and/or the application of the preparation method of the FeCoCr magnetic material in preparing a code wheel material for a magnetic encoder.
The technical scheme provided by the embodiment of the invention has at least the following beneficial effects:
the FeCoCr magnetic material provided by the invention adopts HfO 2 The layer is used as a protective layer and Si substrate/HfO is adopted 2 /FeCoCr/HfO 2 By providing HfO on both sides of the FeCoCr magnetic layer 2 As a protective layer, the defect that Ta element diffuses into a magnetic layer when Ta is adopted as the protective layer in the prior art can be overcome, and further the FeCoCr magnetic material is ensured to have better magnetic performance. Especially, compared with the magnetic material taking Ta as a protective layer in the prior art, the residual magnetism of the FeCoCr magnetic material provided by the invention is doubled, so that the performance requirement of the type of magnetic material in the practical application process can be completely met, and the practical application requirement of a magnetic encoder code wheel can be particularly met.
According to the invention, the preparation method of magnetron sputtering and vacuum annealing is sequentially adopted, and the technological parameters of the magnetron sputtering and vacuum annealing processes are strictly controlled, so that the prepared FeCoCr magnetic material has good performance. The preparation method of the FeCoCr magnetic material provided by the invention has the effects of simple preparation process, easiness in control, high efficiency and low cost.
Detailed Description
In order to make the technical problems, technical solutions and advantages to be solved by the present invention more apparent, the following detailed description will be made with reference to specific embodiments. It will be apparent that the embodiments described below are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
In this embodiment, the specific process for preparing the FeCoCr thin film magnetic material includes:
s1, sequentially ultrasonically cleaning a FeCoCr target material by using acetone and deionized water, and then placing the FeCoCr target material in an oven for drying.
S2, in a magnetron sputtering device, utilizing a magnetron sputtering method to sequentially deposit HfO on the Si substrate 2 Protective layer, feCoCr magnetic layer, hfO 2 And (3) a protective layer. Wherein, in the magnetron sputtering process, the vacuum degree of the sputtering chamber is 3 multiplied by 10 -5 Pa, the pressure of argon gas in the sputtering chamber was 0.3Pa. And sequentially depositing HfO on the Si substrate 2 Protective layer, feCoCr magnetic layer, hfO 2 The deposition time of the protective layer is respectively 60s, 5min and 60s.
And S3, after the deposition step is completed, carrying out vacuum annealing treatment on the material obtained in the step S2. Wherein the annealing temperature is 650At a temperature of 30min, the annealing time is 3×10 in vacuum degree -5 Pa。
The embodiment can prepare the Si substrate/HfO structure 2 (3nm)/FeCoCr(100nm)/HfO 2 (3 nm) FeCoCr thin film magnetic material.
The residual magnetism of the FeCoCr film magnetic material prepared in this example was 7000Oe.
Example 2
In this embodiment, the specific process for preparing the FeCoCr thin film magnetic material includes:
s1, sequentially ultrasonically cleaning a FeCoCr target material by using acetone and deionized water, and then placing the FeCoCr target material in an oven for drying.
S2, in a magnetron sputtering device, utilizing a magnetron sputtering method to sequentially deposit HfO on the Si substrate 2 Protective layer, feCoCr magnetic layer, hfO 2 And (3) a protective layer. Wherein, in the magnetron sputtering process, the vacuum degree of the sputtering chamber is 2 multiplied by 10 -5 Pa, the pressure of argon gas in the sputtering chamber was 0.4Pa. And sequentially depositing HfO on the Si substrate 2 Protective layer, feCoCr magnetic layer, hfO 2 The deposition time of the protective layer is 90s, 7min and 90s respectively.
And S3, after the deposition step is completed, carrying out vacuum annealing treatment on the material obtained in the step S2. Wherein the annealing temperature is 650 ℃, the annealing time is 40min, and the vacuum degree of the annealing environment is 3×10 -5 Pa。
The embodiment can obtain the Si substrate/HfO structure 2 (5nm)/FeCoCr(150nm)/HfO 2 (5 nm) FeCoCr thin film magnetic material.
The residual magnetism of the FeCoCr film magnetic material prepared in the embodiment is 8100Oe.
Example 3
In this embodiment, the specific process for preparing the FeCoCr thin film magnetic material includes:
s1, sequentially ultrasonically cleaning a FeCoCr target material by using acetone and deionized water, and then placing the FeCoCr target material in an oven for drying.
S2, in a magnetron sputtering device, utilizing a magnetron sputtering method to sequentially deposit HfO on the Si substrate 2 Protective layer, feCoCr magnetic layer, hfO 2 And (3) a protective layer. Which is a kind ofIn the magnetron sputtering process, the vacuum degree of the sputtering chamber is 4 multiplied by 10 -5 Pa, the pressure of argon gas in the sputtering chamber was 0.2Pa. And sequentially depositing HfO on the Si substrate 2 Protective layer, feCoCr magnetic layer, hfO 2 The deposition time of the protective layer is 120s, 9min and 120s respectively.
And S3, after the deposition step is completed, carrying out vacuum annealing treatment on the material obtained in the step S2. Wherein the annealing temperature is 550 ℃, the annealing time is 45min, and the vacuum degree of the annealing environment is 2 multiplied by 10 -5 Pa。
The embodiment can obtain the Si substrate/HfO structure 2 (6nm)/FeCoCr(180nm)/HfO 2 (6 nm) FeCoCr thin film magnetic material.
The residual magnetism of the FeCoCr film magnetic material prepared in the embodiment is 8500Oe.
Example 4
In this embodiment, the specific process for preparing the FeCoCr thin film magnetic material includes:
s1, sequentially ultrasonically cleaning a FeCoCr target material by using acetone and deionized water, and then placing the FeCoCr target material in an oven for drying.
S2, in a magnetron sputtering device, utilizing a magnetron sputtering method to sequentially deposit HfO on the Si substrate 2 Protective layer, feCoCr magnetic layer, hfO 2 And (3) a protective layer. Wherein, in the magnetron sputtering process, the vacuum degree of the sputtering chamber is 3 multiplied by 10 -5 Pa, the pressure of argon gas in the sputtering chamber was 0.3Pa. And sequentially depositing HfO on the Si substrate 2 Protective layer, feCoCr magnetic layer, hfO 2 The deposition time of the protective layer is 130s, 10min and 130s respectively.
And S3, after the deposition step is completed, carrying out vacuum annealing treatment on the material obtained in the step S2. Wherein the annealing temperature is 600 ℃, the annealing time is 50min, and the vacuum degree of the annealing environment is 4 multiplied by 10 -5 Pa。
The embodiment can obtain the Si substrate/HfO structure 2 (7nm)/FeCoCr(200nm)/HfO 2 (7 nm) FeCoCr film magnetic material.
The residual magnetism of the FeCoCr film magnetic material prepared in the embodiment is 9100Oe.
Example 5
In this embodiment, the specific process for preparing the FeCoCr thin film magnetic material includes:
s1, sequentially ultrasonically cleaning a FeCoCr target material by using acetone and deionized water, and then placing the FeCoCr target material in an oven for drying.
S2, in a magnetron sputtering device, utilizing a magnetron sputtering method to sequentially deposit HfO on the Si substrate 2 Protective layer, feCoCr magnetic layer, hfO 2 And (3) a protective layer. Wherein, in the magnetron sputtering process, the vacuum degree of the sputtering chamber is 4 multiplied by 10 -5 Pa, the pressure of argon gas in the sputtering chamber was 0.5Pa. And sequentially depositing HfO on the Si substrate 2 Protective layer, feCoCr magnetic layer, hfO 2 The deposition time of the protective layer is 180s, 12min and 180s respectively.
And S3, after the deposition step is completed, carrying out vacuum annealing treatment on the material obtained in the step S2. Wherein the annealing temperature is 700 ℃, the annealing time is 55min, and the vacuum degree of the annealing environment is 3×10 -5 Pa。
The embodiment can obtain the Si substrate/HfO structure 2 (10nm)/FeCoCr(240nm)/HfO 2 (10 nm) FeCoCr thin film magnetic material.
The residual magnetism of the FeCoCr thin film magnetic material prepared in this example was 9500Oe.
Example 6
In this embodiment, the specific process for preparing the FeCoCr thin film magnetic material includes:
s1, sequentially ultrasonically cleaning a FeCoCr target material by using acetone and deionized water, and then placing the FeCoCr target material in an oven for drying.
S2, in a magnetron sputtering device, utilizing a magnetron sputtering method to sequentially deposit HfO on the Si substrate 2 Protective layer, feCoCr magnetic layer, hfO 2 And (3) a protective layer. Wherein, in the magnetron sputtering process, the vacuum degree of the sputtering chamber is 4 multiplied by 10 -5 Pa, the pressure of argon gas in the sputtering chamber was 0.6Pa. And sequentially depositing HfO on the Si substrate 2 Protective layer, feCoCr magnetic layer, hfO 2 The deposition time of the protective layer is 100s, 12min and 100s respectively.
And S3, after the deposition step is completed, carrying out vacuum annealing treatment on the material obtained in the step S2. Wherein the method comprises the steps ofThe annealing temperature is 650 ℃, the annealing time is 60min, and the vacuum degree of the annealing environment is 3 multiplied by 10 -5 Pa。
The embodiment can obtain the Si substrate/HfO structure 2 (6nm)/FeCoCr(220nm)/HfO 2 (6 nm) FeCoCr thin film magnetic material.
The residual magnetism of the FeCoCr film magnetic material prepared in this example was 9350Oe.
Example 7
In this embodiment, the specific process for preparing the FeCoCr thin film magnetic material includes:
s1, sequentially ultrasonically cleaning a FeCoCr target material by using acetone and deionized water, and then placing the FeCoCr target material in an oven for drying.
S2, in a magnetron sputtering device, utilizing a magnetron sputtering method to sequentially deposit HfO on the Si substrate 2 Protective layer, feCoCr magnetic layer, hfO 2 And (3) a protective layer. Wherein, in the magnetron sputtering process, the vacuum degree of the sputtering chamber is 4 multiplied by 10 -5 Pa, the pressure of argon gas in the sputtering chamber was 0.5Pa. And sequentially depositing HfO on the Si substrate 2 Protective layer, feCoCr magnetic layer, hfO 2 The deposition time of the protective layer is 180s, 15min and 180s respectively.
And S3, after the deposition step is completed, carrying out vacuum annealing treatment on the material obtained in the step S2. Wherein the annealing temperature is 650 ℃, the annealing time is 45min, and the vacuum degree of the annealing environment is 5 multiplied by 10 -5 Pa。
The embodiment can obtain the Si substrate/HfO structure 2 (10nm)/FeCoCr(300nm)/HfO 2 (10 nm) FeCoCr thin film magnetic material.
The residual magnetism of the FeCoCr film magnetic material prepared in the embodiment is 11000Oe.
Comparative example 1
In this comparative example, the specific process for preparing a thin film magnetic material having a structure of FeCoCr (100 nm)/Ta (3 nm) comprises:
s1, sequentially ultrasonically cleaning a FeCoCr target material by using acetone and deionized water, and then placing the FeCoCr target material in an oven for drying.
S2, alternately depositing FeCoCr and Ta on the silicon substrate by utilizing a magnetron sputtering method at room temperature, wherein sputtering is performedThe background vacuum degree of the shooting chamber is 3 multiplied by 10 -5 Pa, the chamber gas during sputtering was slightly argon, and the argon pressure was 0.3Pa.
S3, after the deposition is finished, carrying out heat treatment at proper temperature on the film system obtained in the step S2 in a vacuum environment, wherein the vacuum degree of the vacuum environment is 1 multiplied by 10 -5 Pa, the temperature of the heat treatment is 700 ℃, and the heat preservation time is 60min.
The residual magnetism of the FeCoCr (100 nm)/Ta (3 nm) thin film magnetic material obtained in this comparative example was 4550Oe.
While the foregoing is directed to the preferred embodiments of the present invention, it will be appreciated by those skilled in the art that various modifications and adaptations can be made without departing from the principles of the present invention, and such modifications and adaptations are intended to be comprehended within the scope of the present invention.

Claims (9)

1. A FeCoCr magnetic material sequentially provided with a Si base layer, a protective layer, a FeCoCr magnetic layer and a protective layer, wherein the protective layer is composed of HfO 2 The thickness of each protective layer is 3nm-10nm, and the thickness of the FeCoCr magnetic layer is 100nm-300nm;
the FeCoCr magnetic material has a structure of Si basal layer/HfO 2 Protective layer/FeCoCr magnetic layer/HfO 2 And (3) a protective layer.
2. The FeCoCr magnetic material of claim 1, wherein each of the protective layers has a thickness of 5nm-8nm, and the FeCoCr magnetic layer has a thickness of 150nm-280nm.
3. The FeCoCr magnetic material of any of claims 1 or 2, wherein in the FeCoCr magnetic layer, the Fe: co: the weight percentage of Cr is 40-50:25-30:20-30.
4. The FeCoCr magnetic material of claim 3, wherein in the FeCoCr magnetic layer, the Fe: co: the weight percentage of Cr is 45:30:25.
5. A method of producing a FeCoCr magnetic material according to any one of claims 1 to 4, comprising the steps of:
step S1, depositing the protective layer on the Si substrate layer by using a magnetron sputtering device and utilizing a magnetron sputtering method to obtain a first intermediate material;
s2, depositing the FeCoCr magnetic layer on the first intermediate material by utilizing a magnetron sputtering method to obtain a second intermediate material;
step S3, depositing the protective layer on the second intermediate material by utilizing a magnetron sputtering method to obtain a third intermediate layer;
and S4, carrying out vacuum annealing treatment on the third intermediate layer to obtain the FeCoCr magnetic material.
6. The method according to claim 5, wherein the reaction conditions of the magnetron sputtering method in the step S1 to the step S3 include: the pressure is 0.2 Pa-0.7 Pa, and the vacuum degree of the sputtering chamber is 1 multiplied by 10 -5 Pa~4×10 -5 Pa。
7. The method according to claim 5 or 6, wherein the deposition time in the step S1 is 60S to 180S; the deposition time in the step S2 is 5-15 min; the deposition time in the step S3 is 60S-180S.
8. The method according to any one of claims 5 or 6, wherein the reaction conditions for vacuum annealing in step S4 include: the annealing temperature is 550-700 ℃, the annealing time is 30-60 min, and the vacuum degree is 2X 10 -5 Pa~6×10 -5 Pa。
9. Use of a FeCoCr magnetic material according to any one of claims 1-4 and/or a FeCoCr magnetic material according to any one of claims 5-8 in the preparation of a code wheel material for a magnetic encoder.
CN202210623362.0A 2022-06-02 2022-06-02 FeCoCr magnetic material and preparation method and application thereof Active CN115094380B (en)

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