CN106521439B - A kind of preparation method of the adjustable rare earth-transition alloy firm of coercivity - Google Patents
A kind of preparation method of the adjustable rare earth-transition alloy firm of coercivity Download PDFInfo
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- CN106521439B CN106521439B CN201610987929.7A CN201610987929A CN106521439B CN 106521439 B CN106521439 B CN 106521439B CN 201610987929 A CN201610987929 A CN 201610987929A CN 106521439 B CN106521439 B CN 106521439B
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- C—CHEMISTRY; METALLURGY
- C23—COATING 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
- C23C—COATING 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING 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
- C23C—COATING 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
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Abstract
The present invention discloses a kind of preparation method of the adjustable rare-earth transition alloy firm of coercivity, it fits rare earth patch and ferrocobalt target to form combined tessera target, combined tessera target is sputtered using magnetically controlled sputter method, flow by sputtering working gas effectively adjusts the magnetic characteristic of the amorphous alloy film of preparation, realizes the horizontal consecutive variations between vertical and rich transition and rich rare earth composition of film direction of easy axis.The preparation method of the rare-earth transition alloy firm can adjust the magnetic characteristic and coercivity of alloy firm in wide range, meet requirement of the magnetoelectricity recording technique field to material property.
Description
Technical field
The present invention relates to magnetic spin electronics and Magnetographic Technology Material Fields, and in particular to be a kind of to be used for magnetic spin
The preparation method of the adjustable rare earth-transition alloy film material of coercivity of electronic device.
Background technology
Conventional vertical magnetic recording material and laser assisted magnetic recording media amorphous rare earth-transition alloy film material are due to tool
There are big perpendicular magnetic anisotropic and high thermal stability and is constantly subjected to the extensive concern of people.This alloy firm
Coupled in anti-parallel arrangement is presented in the magnetic moment of material rare earth elements (Tb or Dy) and transition element (FeCo) sublattice, causes
There is likely to be a specific compensation point ingredients in this kind of material, correspond to the magnetization of this compensation point composition alloy film
Intensity is zero but coercivity is infinitely great.It is general for the rare earth-transition alloy firm ingredient of the vertical film surface of direction of easy axis
Near compensation point ingredient.It is brilliant to be more than transition element for the magnetic moment of alloy film material rare earth elements sublattice when room temperature
On the contrary then alloy firm ingredient is rich rare earth to the magnetic moment of lattice, then be richness transition.
Currently, with the fast development of this emerging field of magnetic spin electronics, ferrimagnetism rare earth-transition alloy firm
Material drives domain wall motion etc. to obtain new application in high density, the vertical magnetic random memory part of low energy consumption and electric current.
Different from the big coercivity of the room temperature required in perpendicular magnetic recording, high-density current driving spin storage requires this dilute with logical device
Soil-Transition-metal Alloys film has moderate perpendicular coercive force reduces power consumption with the current density for reducing current induced magnetization overturning.
Therefore it finds and prepares the preparation method with the coercitive rare earth-transition alloy firm of suitable vertical, in current magnetic spin electronics
It learns the novel informations memory areas such as the direct induced magnetization overturning of device especially electric current to be of great significance, and is possible to generate
Huge economic benefits.
The coercivity size of rare earth-transition alloy firm is directly related with its ingredient.By changing film middle rare earth and mistake
The ingredient of element is crossed than different coercivitys may be implemented.In practical application, such rare earth-transition alloy firm generally by
Direct current either radio-frequency sputtering method prepare thin film composition can by variation combined tessera target patch location and ratio or
Changed using the ternary alloy three-partalloy target of heterogeneity ratio.But above method be required for destroy vacuum change target, it is inconvenient,
Long preparation period, moreover, using heterogeneity alloys target it is expensive.
Invention content
It is at low cost the purpose of the present invention is to provide a kind of preparation method of the adjustable rare earth-transition alloy firm of coercivity
It is honest and clean, short preparation period.The preparation method can be realized thin in the case where not destroying vacuum by simple sputtering process control
The consecutive variations of membrane property, facilitate the vertical alloy firm of adjustment at branch, expansion prepares the coercivity range of film, conveniently seeks
It looks for suitable coercitive rare earth-transition race alloy firm and explores the optimum performance of alloy firm into branch.
In order to achieve the above objectives, solution of the invention is：
A kind of preparation method of the adjustable rare earth-transition alloy firm of coercivity, includes the following steps：
(1) multi-disc is symmetrically attached to purity >=99.9% in the rare earth patch of purity >=99.9% of isosceles triangle
Ferrocobalt target on, formed sputtering combined tessera target, the rare earth patch be Tb patches or Dy patches, the rare earth
The apex angle of patch be 15~40 °, the 70~90% of the radius length of a length of ferrocobalt target of waist of the rare earth patch；
(2) using the combined tessera target as the target of magnetron sputtering, it is fixed on the sputtering target stand of magnetron sputtering chamber
On；
(3) by after cleaning, drying substrate placement be fixed on the chip bench of magnetron sputtering chamber, adjustment target-substrate distance be 4~
8cm；
(4) sputtering vacuum chamber is reached into vacuum degree 1 × 10-5Pa is hereinafter, the argon gas for being passed through purity >=99.99% is made
For working gas, the charge flow rate of argon gas is controlled within the scope of 25~100sccm；
(5) under conditions of sputtering 0.2~1.0Pa of operating air pressure, to 10~30min of the combined tessera target pre-sputtering；
(6) chip bench 5~15 circle of rotation per minute is adjusted, chip bench is opened and sputters the baffle between target stand, with 1.5~
5W/cm2Sputtering power density sputter the combined tessera target, sputtering time is 1~20min, obtains thick dilute of 20~400nm
Soil-Transition-metal Alloys film.
The quantity of the rare earth patch is 3~6, during each rare earth patch is with the center of circle of the ferrocobalt target
Heart point is distributed on the ferrocobalt target.
After adopting the above technical scheme, a kind of preparation method of the adjustable rare earth-transition alloy firm of coercivity of the present invention, tool
There is following advantage：When combined tessera target sputter coating, using the charge flow rate for adjusting work argon gas, rare earth-transition alloy is adjusted
Deviation of the ingredient of film relative to compensation point ingredient, realizes the consecutive variations of magnetic characteristic, reaches rare earth-transition alloy firm
Coercivity adjustable purpose in wider range；The quantity that rare earth patch on alloy target material need not be increased or decreased is not being broken
Bad vacuum or change target in the case of, directly by change working gas charge flow rate adjustment prepare film at split-phase
For the deviation of compensation point ingredient, realize that film direction of easy axis is horizontal between vertical and rich transition and rich rare earth composition
Flexibly variation facilitates the coercivity of adjustment alloy firm, can prepare coercivity adjustable alloy firm and spy in wide range
Rope optimum performance ingredient section, meets requirement of the magnetoelectricity recording technique field to material property.
Description of the drawings
Fig. 1 is the TbFeCo alloy film XRD results of 100nm thickness on single crystalline Si (100) substrate；
Fig. 2 is that a) sputtering prepares the unusual magnetoelectricity Hall effect loop line of TbFeCo alloy film, b under different gas flow)
Coercivity and gas flow change curve, dotted line indicates corresponding charge flow rate when the preparation of compensation point composition alloy film in figure
Between 50 and 65sccm；
Fig. 3 is the DyFeCo alloy firm XRD results of 100nm thickness on single crystalline Si (100) substrate；
Fig. 4 is that a) sputtering prepares the unusual magnetoelectricity Hall effect loop lines of DyFeCo alloy firms, b under different gas flow)
Coercivity and gas flow change curve, dotted line indicates corresponding charge flow rate when the preparation of compensation point composition alloy film in figure
Between 50 and 60sccm.
Specific implementation mode
In order to further explain the technical solution of the present invention, being explained in detail the present invention below by specific embodiment
It states.
Embodiment one
One, the preparation of thin-film material
A kind of preparation method of the adjustable rare earth-transition alloy firm of coercivity, includes the following steps：
(1) it is 1 inch three pieces to be attached to radius in the Tb patches of the high-purity (purity 99.95%) of isosceles triangle
On the ferrocobalt target of high-purity (purity 99.9%), the combined tessera target of sputtering is formed, each Tb patch is closed with iron cobalt
Point is distributed on ferrocobalt target centered on the center of circle of gold target, and the apex angle of Tb patches is 28 °, a length of 2cm of waist of Tb patches, thickness
For 2mm；
(2) it using combined tessera target as the target of magnetron sputtering, is fixed on the sputtering target stand of magnetron sputtering chamber；
(3) it with single crystalline Si (100) for substrate, is dried after being cleaned by ultrasonic successively with acetone, alcohol, isopropanol to substrate, it will
Substrate placement after drying and processing is fixed on the chip bench of magnetron sputtering chamber, and adjustment target-substrate distance is 5.5cm；
(4) it is 1 × 10 sputtering vacuum chamber to be reached vacuum degree-5Pa, being passed through the argon gas of high-purity, (purity is
99.999%) it is used as working gas, controls the charge flow rate of argon gas within the scope of 35~100sccm；
(5) degree that adjustment slide valve is closed keeps sputtering operating air pressure stable and maintains 0.2Pa, to combined tessera target
Pre-sputtering 20min；
(6) chip bench 10 circle of rotation per minute is adjusted, chip bench is opened and sputters the baffle between target stand, with 4W/cm2's
Sputtering power density sputters combined tessera target, sputtering time 4min, and sputtering finishes postcooling to get thick to 100nm
TbFeCo alloy film.
Two, structure and performance test
The XRD characterization of TbFeCo alloy film has no thin film diffraction as shown in Figure 1, in addition to substrate Si (400) peak in figure
Peak shows that the alloy firm is non crystalline structure.
The magnetic characteristic of TbFeCo alloy film characterizes as shown in Fig. 2, sputtering prepares TbFeCo alloy under different gas flow
The unusual magnetoelectricity Hall effect loop line of film shows：The easy magnetic of the alloy firm prepared when the charge flow rate of argon gas is 35sccm
It is level to change direction, and the direction of easy axis of the alloy firm prepared when the charge flow rate of argon gas is 50sccm is between horizontal and vertical
Between straight, ingredient is rich transition；When the charge flow rate of argon gas is between 65~100sccm, the alloy firm of preparation it is easy
The direction of magnetization is vertical, and ingredient is rich rare earth.Thin film coercitive force shows with gas flow change curve：By changing argon flow amount
The coercivity of the alloy firm of preparation may be implemented in the wide variation between 0~8kOe.
Embodiment two
One, the preparation of thin-film material
A kind of preparation method of the adjustable rare earth-transition alloy firm of coercivity, includes the following steps：
(1) it is 1 inch three pieces to be attached to radius in the Dy patches of the high-purity (purity 99.95%) of isosceles triangle
On the ferrocobalt target of high-purity (purity 99.9%), the combined tessera target of sputtering is formed, each Dy patch is closed with iron cobalt
Point is distributed on ferrocobalt target centered on the center of circle of gold target, and the apex angle of Dy patches is 28 °, a length of 2cm of waist of Dy patches, thickness
For 2mm；
(2) it using combined tessera target as the target of magnetron sputtering, is fixed on the sputtering target stand of magnetron sputtering chamber；
(3) it with single crystalline Si (100) for substrate, is dried after being cleaned by ultrasonic successively with acetone, alcohol, isopropanol to substrate, it will
Substrate placement after drying and processing is fixed on the chip bench of magnetron sputtering chamber, and adjustment target-substrate distance is 5.5cm；
(4) it is 1 × 10 sputtering vacuum chamber to be reached vacuum degree-5Pa, being passed through the argon gas of high-purity, (purity is
99.999%) it is used as working gas, controls the charge flow rate of argon gas within the scope of 35~100sccm；
(5) degree that adjustment slide valve is closed keeps sputtering operating air pressure stable and maintains 0.2Pa, to combined tessera target
Pre-sputtering 20min；
(6) chip bench 10 circle of rotation per minute is adjusted, chip bench is opened and sputters the baffle between target stand, with 3.2W/cm2
Sputtering power density sputter combined tessera target, sputtering time 5min, sputtering finishes postcooling to get thick to 100nm
DyFeCo alloy firms.
Two, structure and performance test
The XRD characterization of DyFeCo alloy firms has no thin film diffraction as shown in figure 3, in addition to substrate Si (400) peak in figure
Peak shows that the alloy firm is non crystalline structure.
The magnetic characteristic of DyFeCo alloy firms characterizes as shown in figure 4, sputtering prepares DyFeCo alloys under different gas flow
The unusual magnetoelectricity Hall effect loop line of film shows：The easy magnetic of the alloy firm prepared when the charge flow rate of argon gas is 40sccm
It is level to change direction, and the direction of easy axis of the alloy firm prepared when the charge flow rate of argon gas is 50sccm is between horizontal and vertical
Between straight, ingredient is rich transition；When argon gas charge flow rate between 60 between 100sccm, the easy magnetic of the alloy firm of preparation
It is vertical to change direction, and ingredient is rich rare earth.Thin film coercitive force shows with gas flow change curve：By changing argon flow amount system
The coercivity of standby alloy firm may be implemented in the wide variation between 0~4.3kOe.
Embodiment three
A kind of preparation method of the adjustable rare earth-transition alloy firm of coercivity, includes the following steps：
(1) it is 1 inch three pieces to be attached to radius in the Dy patches of the high-purity (purity 99.95%) of isosceles triangle
On the ferrocobalt target of high-purity (purity 99.9%), the combined tessera target of sputtering is formed, each Dy patch is closed with iron cobalt
Point is distributed on ferrocobalt target centered on the center of circle of gold target, and the apex angle of Dy patches is 28 °, a length of 2cm of waist of Dy patches, thickness
For 2mm；
(2) it using combined tessera target as the target of magnetron sputtering, is fixed on the sputtering target stand of magnetron sputtering chamber；
(3) it with single crystalline Si (100) for substrate, is dried after being cleaned by ultrasonic successively with acetone, alcohol, isopropanol to substrate, it will
Substrate placement after drying and processing is fixed on the chip bench of magnetron sputtering chamber, and adjustment target-substrate distance is 5.5cm；
(4) it is 1 × 10 sputtering vacuum chamber to be reached vacuum degree-5Pa, being passed through high purity argon, (purity is
99.999%) it is used as working gas, controls the charge flow rate of argon gas in 60sccm；
(5) degree that adjustment slide valve is closed keeps sputtering operating air pressure stable and maintains 0.2Pa, to combined tessera target
Pre-sputtering 20min；
(6) chip bench 10 circle of rotation per minute is adjusted, chip bench is opened and sputters the baffle between target stand, with 3.2W/cm2
Sputtering power density sputter combined tessera target, sputtering time is 1~20min, sputtering finish postcooling to get to 20~
The DyFeCo alloy firms of 400nm thickness.
In the present embodiment, by controlling sputtering time, the DyFeCo alloy firms of different-thickness can be obtained, sputtering time is got over
Long, the thickness of film is bigger, but is that 1~10min obtains the alloy firm that thickness is 20~200nm and is advisable with sputtering time.
Rare earth patch and ferrocobalt target in the various embodiments described above are commercially available on the market, only need to be according to purity
It is required that purchase.
The product form and style of above-described embodiment and schema and the non-limiting present invention, any technical field it is common
The appropriate changes or modifications that technical staff does it all should be regarded as the patent category for not departing from the present invention.
Claims (2)
1. a kind of preparation method of the adjustable rare earth-transition alloy firm of coercivity, it is characterised in that：Include the following steps：
(1) multi-disc is symmetrically attached to purity >=99.9% in the rare earth patch of purity >=99.9% of isosceles triangle
On ferrocobalt target, the combined tessera target of sputtering is formed, the rare earth patch is Tb patches or Dy patches, the rare earth patch
The apex angle of piece be 15~40 °, the 70~90% of the radius length of a length of ferrocobalt target of waist of the rare earth patch；
(2) it using the combined tessera target as the target of magnetron sputtering, is fixed on the sputtering target stand of magnetron sputtering chamber；
(3) the substrate placement after cleaning, drying is fixed on the chip bench of magnetron sputtering chamber, adjustment target-substrate distance is 4~8cm；
(4) vacuum chamber will be sputtered, the indoor pressure of sputtering vacuum is made to be less than 1 × 10-5Pa is passed through purity >=99.99%
Argon gas as working gas, control the charge flow rate of argon gas within the scope of 25~100sccm；
(5) under conditions of sputtering 0.2~1.0Pa of operating air pressure, to 10~30min of the combined tessera target pre-sputtering；
(6) chip bench 5~15 circle of rotation per minute is adjusted, chip bench is opened and sputters the baffle between target stand, with 1.5~5W/
cm2Sputtering power density sputter the combined tessera target, sputtering time is 1~20min, obtains the rare earth-of 20~400nm thickness
Transition-metal Alloys film.
2. a kind of preparation method of the adjustable rare earth-transition alloy firm of coercivity according to claim 1, feature exist
In：The quantity of the rare earth patch is 3~6, each rare earth patch point centered on the center of circle of the ferrocobalt target
It is distributed on the ferrocobalt target.
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107190242A (en) * | 2017-05-12 | 2017-09-22 | 华侨大学 | A kind of preparation method with a wide range of adjustable coercivity nano thickness rare-earth transition alloy firm |
| CN107275073A (en) * | 2017-06-09 | 2017-10-20 | 华侨大学 | A kind of preparation method of the adjustable nano thickness GdFeCo alloy firms of vertical magnetic characteristic |
| CN107523796B (en) * | 2017-07-21 | 2019-07-05 | 华侨大学 | A kind of preparation method of the rare earth-transition alloy composite materials with wall |
| CN107611257B (en) * | 2017-07-21 | 2019-11-12 | 华侨大学 | A kind of vertically negative artificial magnetic coupling arrangement material of coercivity and preparation method thereof |
| CN107587109B (en) * | 2017-08-21 | 2019-06-04 | 华侨大学 | Composite multi-layer membrane structure with high vertical off setting field and big overturning field platform |
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| EP0309022A1 (en) * | 1987-09-14 | 1989-03-29 | Koninklijke Philips Electronics N.V. | Method of producing thin magnetic metallic layers having a low thermal coefficient of expansion |
| US6117282A (en) * | 1997-09-23 | 2000-09-12 | Kuo; Po-Cheng | Method of producing amorphous Co-Tb magnetic recording thin films |
| CN103820765A (en) * | 2014-03-22 | 2014-05-28 | 沈阳中北真空设备有限公司 | Composite coating equipment and manufacturing method for neodymium iron boron rare-earth permanent magnetic device |
| CN105755441A (en) * | 2016-04-20 | 2016-07-13 | 中国科学院宁波材料技术与工程研究所 | Method for diffusing permeation of heavy rare earth through magnetron sputtering method to improve coercivity of sintered neodymium iron boron |
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| EP0309022A1 (en) * | 1987-09-14 | 1989-03-29 | Koninklijke Philips Electronics N.V. | Method of producing thin magnetic metallic layers having a low thermal coefficient of expansion |
| US6117282A (en) * | 1997-09-23 | 2000-09-12 | Kuo; Po-Cheng | Method of producing amorphous Co-Tb magnetic recording thin films |
| CN103820765A (en) * | 2014-03-22 | 2014-05-28 | 沈阳中北真空设备有限公司 | Composite coating equipment and manufacturing method for neodymium iron boron rare-earth permanent magnetic device |
| CN105755441A (en) * | 2016-04-20 | 2016-07-13 | 中国科学院宁波材料技术与工程研究所 | Method for diffusing permeation of heavy rare earth through magnetron sputtering method to improve coercivity of sintered neodymium iron boron |
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