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CN110016649A - A kind of coercitive method of rare earth-transition alloy firm adjusting the ion containing Gd - Google Patents

A kind of coercitive method of rare earth-transition alloy firm adjusting the ion containing Gd Download PDF

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Publication number
CN110016649A
CN110016649A CN201910395958.8A CN201910395958A CN110016649A CN 110016649 A CN110016649 A CN 110016649A CN 201910395958 A CN201910395958 A CN 201910395958A CN 110016649 A CN110016649 A CN 110016649A
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China
Prior art keywords
rare earth
alloy firm
transition alloy
adjusting
ion containing
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CN201910395958.8A
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Chinese (zh)
Inventor
王可
马杰
王亚宏
张明智
刘剑
马善农
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East China Institute of Technology
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East China Institute of Technology
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Priority to CN201910395958.8A priority Critical patent/CN110016649A/en
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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
    • 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
    • C23C14/18Metallic material, boron or silicon on other inorganic substrates
    • 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
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00Apparatus 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
    • H01F41/14Apparatus 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
    • H01F41/18Apparatus 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
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00Apparatus 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
    • H01F41/14Apparatus 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
    • H01F41/18Apparatus 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
    • H01F41/183Sputtering targets therefor

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Inorganic Chemistry (AREA)
  • Physical Vapour Deposition (AREA)
  • Thin Magnetic Films (AREA)

Abstract

The invention discloses a kind of coercitive method of rare earth-transition alloy firm for adjusting the ion containing Gd, the problem of being to solve the rare earth-transition alloy firm of the existing ion containing Gd.Specific step is as follows: step 1 by the present invention, Gd patch and mosaic target is formed composition target, then composition target is put into the target position of vacuum sputtering room, substrate is fixed on the chip bench of vacuum sputtering room, is passed through working gas to vacuum sputtering room;Step 2, the sputtering buffering bottom on substrate;Step 3 sputters rare earth-transition alloy firm of the growth of vertical containing Gd on buffering bottom;Step 4, the sputtering protection top layer on the rare earth-transition alloy firm containing Gd.Preparation method of the present invention is simple, reproducible, low in cost;The variation that alloy firm coercivity is up to 200% or more may be implemented in the present invention within the scope of certain thickness, promotes the precession and reversion of alloy firm magnetic moment, to realize that reliable spin moment device provides simple structure.

Description

A kind of coercitive method of rare earth-transition alloy firm adjusting the ion containing Gd
Technical field
It is specifically a kind of to adjust the dilute of the ion containing Gd the present invention relates to magnetic spin electronics and recording technique Material Field Soil-Transition-metal Alloys thin film coercitive force method.
Background technique
With the fast development of magnetic spin electronics, Ferrimagnetic rare earth-transition alloy film material is in high density, low energy consumption Vertical magnetic random memory part and electric current driving domain wall motion etc. obtain new application.With contain Tb (terbium) or Dy (dysprosium) ion Ferrimagnetic (Tb, Dy)-transition (Fe, Co) alloy firm compare, the rare earth-transition alloy of the corresponding Gd of state containing S (gadolinium) ion Film normal anisotropy usually can be more than small an order of magnitude.Meanwhile amorphous Ferrimagnetic rare earth-transition containing Gd (Fe, Co) closes Gold thin film material is with the shadow that minimum magnetocrystalline anisotropy can be ignored and high magnetoelastic coupling coefficient leads to stress to its magnetic characteristic Sound is fairly obvious.Since rare earth element is oxidizable, rare earth-transition alloy needs protective layer to avoid directly contacting with air.We Selecting has the non-magnetic heavy metal material of strong Quantum geometrical phase as protection top layer, by simply changing heavy metal top layer thickness Suitable stress variation is generated within the scope of certain thickness achieves that the coercivity of the alloy firm of rare earth-transition containing Gd significantly Variation.
Currently, the vertical rare earth-transition alloy firm of the small Ferrimagnetic of saturation magnetization and have strong Quantum geometrical phase Non-magnetic heavy metal formed hetero-junctions be also spintronics research field one of hot spot.Have at structure median surface by force certainly Rotation orbit coupling heavy metal layer generates spin polarized current by logic gates and is injected into neighbouring magnetosphere, can promote film The precession and reversion of magnetic moment, to realize that reliable spin moment device provides simpler structure.Current research work is all It is to be used based on non-magnetic heavy metal/ferromagnetic thin film structure or non-magnetic heavy metal as the buffering bottom in double-layer structure, thereon Regrowth ferrimagnetic films (such as Z.Zhao, Appl.Phys.Lett., 106 (13), 132404 (2015) and W.S.Ham etc., Appl.Phys.Lett.110,242405 (2017)), the using effect of this structure is unsatisfactory.
Summary of the invention
A kind of rare earth-transition alloy firm for being designed to provide adjusting ion containing Gd of the embodiment of the present invention is coercitive Method, to solve the problems mentioned in the above background technology.
To achieve the above object, the embodiment of the present invention provides the following technical solutions:
A kind of coercitive method of rare earth-transition alloy firm adjusting the ion containing Gd, the specific steps are as follows:
High-purity Gd patch and mosaic target are formed composition target, then composition target are put into the target of vacuum sputtering room by step 1 Position, substrate is fixed on the chip bench of vacuum sputtering room, is passed through working gas to vacuum sputtering room;
Step 2, the sputtering buffering bottom on substrate;
Step 3 sputters rare earth-transition alloy firm of the growth of vertical containing Gd on buffering bottom;
Step 4, sputtering protects top layer to get finished product is arrived on the rare earth-transition alloy firm containing Gd.
As further embodiment of the embodiment of the present invention: substrate carries out cleaning and drying and processing before being fixed on chip bench.
As further embodiment of the embodiment of the present invention: working gas is high purity argon, the vacuum degree of vacuum sputtering room It is 1 × 10-5Pa is hereinafter, guarantee working environment.
As further embodiment of the embodiment of the present invention: mosaic target is using any one in iron, cobalt or ferrocobalt Material production.
As further embodiment of the embodiment of the present invention: buffering bottom uses metal buffer bottom, and protection top layer is using gold Belong to protection top layer.
As further embodiment of the embodiment of the present invention: buffering bottom is tantalum layer, palladium layers or platinum layer with protection top layer In any one.
As further embodiment of the embodiment of the present invention: the thickness of buffering bottom and protection top layer is 3-20nm.
As further embodiment of the embodiment of the present invention: the rare earth-transition alloy firm containing Gd be Gd- (Fe, Co) or GdFe (iron) Co (cobalt) material, for Gd element (atomic ratio) ingredient between 23.5-26%, film easy axis direction is vertical film surface.
As further embodiment of the embodiment of the present invention: the rare earth-transition alloy firm containing Gd with a thickness of 10-25nm.
Compared with prior art, the beneficial effect of the embodiment of the present invention is:
Preparation method of the present invention is simple, reproducible, low in cost;
The present invention answers masterpiece to what bottom alloy generated as protection top layer using with strong Quantum geometrical phase heavy metal With the variation that alloy firm coercivity is up to 200% or more may be implemented within the scope of certain thickness;Meanwhile structure median surface Place's metal layer generates spin polarized current by logic gates and is injected into adjacent alloys layers, promotes alloy firm magnetic moment Precession and reversion can be applied to magnetoelectricity, magnetic sensor device and surpass to realize that reliable spin moment device provides simple structure In fast record field.
Detailed description of the invention
Fig. 1 is that adjust the structure that the coercitive method of rare earth-transition alloy firm of the ion containing Gd obtains be Si/Ta The unusual magnetoelectricity Hall effect hysteresis loop figure of (5nm)/GdFeCo (20nm)/Ta (t=3~20nm) material.Unusual magnetoelectricity is suddenly Your effect is one of the powerful measure of thin magnetic film especially ultrathin film hysteresis measurement.Extraordinary Hall effect is from suddenly In your effect with intrinsic magnetism of material related part, abnormality Hall voltage is directly proportional to the intensity of magnetization of sample, only needs to survey The unusual Hall voltage of sample and the curve in magnetic field are measured, the hysteresis loop of sample can be obtained.
Fig. 2 is that adjust the structure that the coercitive method of rare earth-transition alloy firm of the ion containing Gd obtains be Si/Ta The unusual magnetoelectricity Hall effect hysteresis loop figure of (5nm)/GdFeCo (22nm)/Ta (t=3~16nm) material.
Specific embodiment
The technical solution of the patent is explained in further detail With reference to embodiment.
Embodiment 1
A kind of coercitive method of rare earth-transition alloy firm adjusting the ion containing Gd, the specific steps are as follows:
High-purity Gd patch and iron target are formed composition target, then composition target are put into the target position of vacuum sputtering room by step 1, Substrate is fixed on the chip bench of vacuum sputtering room, is passed through high purity argon, the vacuum of vacuum sputtering room to vacuum sputtering room Degree is 5.2 × 10-6Pa;
Step 2, on substrate sputtering buffering bottom, buffering bottom use tantalum layer, buffer bottom with a thickness of 10nm;
Step 3 sputters rare earth-transition alloy firm of the growth of vertical containing Gd, rare earth-mistake containing Gd on buffering bottom Crossing alloy firm is Gd- (Fe, Co) material;
Step 4, the sputtering protection top layer on the rare earth-transition alloy firm containing Gd, protection top layer use palladium layers, protection Top layer with a thickness of 15nm to get arrive finished product.
Embodiment 2
A kind of coercitive method of rare earth-transition alloy firm adjusting the ion containing Gd, the specific steps are as follows:
High-purity Gd patch and ferrocobalt target are formed composition target, then composition target are put into vacuum sputtering room by step 1 Target position, substrate is fixed on the chip bench of vacuum sputtering room, substrate, which is fixed on before chip bench, carries out cleaning and drying and processing, It is passed through working gas to vacuum sputtering room, the vacuum degree of vacuum sputtering room is 3.6 × 10-6Pa is hereinafter, guarantee working environment;
Step 2, the sputtering buffering bottom on substrate;
Step 3 sputters rare earth-transition alloy firm of the growth of vertical containing Gd, rare earth-mistake containing Gd on buffering bottom Alloy firm GdFeCo material is crossed, for Gd element (atomic ratio) ingredient between 23.5-26%, film easy axis direction is vertical film surface, Rare earth-transition alloy firm containing Gd with a thickness of 24nm;
Step 4, sputtering protects top layer to get finished product is arrived on the rare earth-transition alloy firm containing Gd.
Embodiment 3
A kind of coercitive method of rare earth-transition alloy firm adjusting the ion containing Gd, the specific steps are as follows:
High-purity Gd patch and mosaic target are formed composition target, then composition target are put into the target of vacuum sputtering room by step 1 Position, substrate is fixed on the chip bench of vacuum sputtering room, and substrate carries out cleaning and drying and processing, Xiang Zhen before being fixed on chip bench Empty sputtering chamber is passed through working gas;
Step 2, the sputtering buffering bottom on substrate;
Step 3 sputters rare earth-transition alloy firm of the growth of vertical containing Gd on buffering bottom;
Step 4, sputtering protects top layer to get finished product is arrived on the rare earth-transition alloy firm containing Gd.
Finished product prepared by embodiment 3 is Si/Ta (5nm)/GdFeCo (20nm)/Ta (t=3~20nm) material, to the material Material carries out magnetization test, the result is shown in Figure 1.
From figure 1 it appears that the thickness t of protection top layer Ta changes to 20nm from 3nm.Before sputtering GdFeCo, first in Si The Ta of pre-sputtering 5nm is as buffering bottom on substrate.Sputtering prepare GdFeCo film with a thickness of 20nm, the atomic ratio of Gd element Ingredient is 24%, and magnetic characteristic shows as rich transition.When top layer Ta is 3nm, sample coercivity minimum 22.8Oe, top layer Ta are Sample coercivity is up to 74.5Oe when 16nm, and coercivity increases 226.7%.
Embodiment 4
A kind of coercitive method of rare earth-transition alloy firm adjusting the ion containing Gd, the specific steps are as follows:
High-purity Gd patch and mosaic target are formed composition target, then composition target are put into the target of vacuum sputtering room by step 1 Position, substrate is fixed on the chip bench of vacuum sputtering room, is passed through working gas to vacuum sputtering room, working gas is high-purity Argon gas, the vacuum degree of vacuum sputtering room are 3.2 × 10-6Pa guarantees working environment;
Step 2, the sputtering buffering bottom on substrate;
Step 3 sputters rare earth-transition alloy firm of the growth of vertical containing Gd on buffering bottom;
Step 4, sputtering protects top layer to get finished product is arrived on the rare earth-transition alloy firm containing Gd.
Finished product prepared by embodiment 4 is Si/Ta (5nm)/GdFeCo (22nm)/Ta (t=3~16nm) material, to the material Material carries out magnetization test, as a result sees Fig. 2.
From figure 2 it can be seen that the thickness t of protection top layer Ta changes to 16nm from 3nm.Before sputtering GdFeCo, first in Si The Ta of pre-sputtering 5nm is as buffering bottom on substrate.Sputtering prepare GdFeCo film with a thickness of 22nm, the atomic ratio of Gd element Ingredient is 24.5%, and magnetic characteristic shows as rich transition.Sample coercivity minimum 54.2Oe, top layer Ta when top layer Ta is 3nm Sample coercivity is up to 197.8Oe when for 12nm, and coercivity increases 264.9%.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.No It should treat any reference in the claims as limiting the claims involved.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should It considers the specification as a whole, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art The other embodiments being understood that.

Claims (9)

1. a kind of coercitive method of rare earth-transition alloy firm for adjusting the ion containing Gd, which is characterized in that specific steps are such as Under:
High-purity Gd patch and mosaic target are formed composition target, then composition target are put into the target position of vacuum sputtering room by step 1, will Substrate is fixed on the chip bench of vacuum sputtering room, is passed through working gas to vacuum sputtering room;
Step 2, the sputtering buffering bottom on substrate;
Step 3 sputters rare earth-transition alloy firm of the growth of vertical containing Gd on buffering bottom;
Step 4, sputtering protects top layer to get finished product is arrived on the rare earth-transition alloy firm containing Gd.
2. the rare earth-transition alloy firm coercitive method according to claim 1 for adjusting the ion containing Gd, feature exist In the substrate carries out cleaning and drying and processing before being fixed on chip bench.
3. the rare earth-transition alloy firm coercitive method according to claim 1 for adjusting the ion containing Gd, feature exist In the working gas is high purity argon, and the vacuum degree of vacuum sputtering room is 1 × 10-5Pa or less.
4. the rare earth-transition alloy firm coercitive method according to claim 1 or 3 for adjusting the ion containing Gd, special Sign is that the mosaic target is using any one material production in iron, cobalt or ferrocobalt.
5. the rare earth-transition alloy firm coercitive method according to claim 1 for adjusting the ion containing Gd, feature exist In the buffering bottom uses metal buffer bottom, and protection top layer uses metal coating top layer.
6. the rare earth-transition alloy firm coercitive method according to claim 5 for adjusting the ion containing Gd, feature exist In the buffering bottom and any one that protection top layer is in tantalum layer, palladium layers or platinum layer.
7. the rare earth-transition alloy firm coercitive method according to claim 1 for adjusting the ion containing Gd, feature exist In the thickness of the buffering bottom and protection top layer is 3-20nm.
8. the rare earth-transition alloy firm coercitive method according to claim 1 for adjusting the ion containing Gd, feature exist In the rare earth-transition alloy firm containing Gd is Gd- (Fe, Co) or GdFeCo material.
9. the coercitive method of rare earth-transition alloy firm of adjusting ion containing Gd according to claim 1 or 8, special Sign is, the rare earth-transition alloy firm containing Gd with a thickness of 10-25nm.
CN201910395958.8A 2019-05-14 2019-05-14 A kind of coercitive method of rare earth-transition alloy firm adjusting the ion containing Gd Pending CN110016649A (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01136947A (en) * 1987-11-20 1989-05-30 Mitsui Petrochem Ind Ltd Amorphous alloy thin film
US20030049495A1 (en) * 2001-07-06 2003-03-13 Yasushi Sakai Perpendicular magnetic recording medium and fabrication method thereof
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
CN107365971A (en) * 2017-08-23 2017-11-21 华侨大学 A kind of rare-earth transition alloy firm with high vertical exchange coupled field and preparation method thereof
CN107611257A (en) * 2017-07-21 2018-01-19 华侨大学 Artificial magnetic coupling arrangement material of a kind of vertically negative coercivity and preparation method thereof
US20180166628A1 (en) * 2016-12-14 2018-06-14 Korea University Research And Business Foundation Alloy thin films exhibiting perpendicular magnetic anisotropy

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01136947A (en) * 1987-11-20 1989-05-30 Mitsui Petrochem Ind Ltd Amorphous alloy thin film
US20030049495A1 (en) * 2001-07-06 2003-03-13 Yasushi Sakai Perpendicular magnetic recording medium and fabrication method thereof
US20180166628A1 (en) * 2016-12-14 2018-06-14 Korea University Research And Business Foundation Alloy thin films exhibiting perpendicular magnetic anisotropy
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
CN107611257A (en) * 2017-07-21 2018-01-19 华侨大学 Artificial magnetic coupling arrangement material of a kind of vertically negative coercivity and preparation method thereof
CN107365971A (en) * 2017-08-23 2017-11-21 华侨大学 A kind of rare-earth transition alloy firm with high vertical exchange coupled field and preparation method thereof

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Application publication date: 20190716