CN102779533A - FeRhPt composite film adjustable in phase transition temperature and preparation method of FeRhPt composite film - Google Patents

FeRhPt composite film adjustable in phase transition temperature and preparation method of FeRhPt composite film Download PDF

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CN102779533A
CN102779533A CN2012102515696A CN201210251569A CN102779533A CN 102779533 A CN102779533 A CN 102779533A CN 2012102515696 A CN2012102515696 A CN 2012102515696A CN 201210251569 A CN201210251569 A CN 201210251569A CN 102779533 A CN102779533 A CN 102779533A
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ferhpt
preparation
phase transition
transition temperature
composite film
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CN102779533B (en
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陆伟
陈哲
何晨冲
严彪
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Tongji University
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Tongji University
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Abstract

The invention relates to the field of magnetic materials and particularly discloses a FeRhPt composite film adjustable in phase transition temperature and a preparation method of the FeRhPt composite film. The FeRhPt composite film adjustable in phase transition temperature comprises a monocrystal MgO substrate and a (FeRh)100-XPtX alloy film on the monocrystal MgO substrate, wherein the value range of x is 0<x<20. Epitaxial growth and vertical orientation of the FeRhPt film is realized by means of the monocrystal MgO substrate, and a perfect CsCl ordered structure is obtained. Further, the FeRhPt composite film is induced by means of annealing treatment to complete ordering to enable materials to have antiferromagnetic/ferromagnetic phase transition, and a series of FeRhPt composite films adjustable in phase transition temperature can be obtained by means of preparation. The FeRhPt composite film adjustable in phase transition temperature and the preparation method of the FeRhPt composite film have the advantages of simple preparation method, fine material performances and the like, and the method is applicable to preparation of FeRhPt composite films adjustable in phase transition temperature.

Description

FeRhPt laminated film that a kind of phase transition temperature is adjustable and preparation method thereof
Technical field
The present invention relates to field of magnetic material, specifically disclose adjustable FeRhPt laminated film of a kind of phase transition temperature and preparation method thereof.
Background technology
Existing research has been found that (330K～350K) the FeRh alloy has a first order phase change from antiferromagnetic to ferromagnetic in a lower temperature range.It is relevant that this changes the CsCl type body-centered cubic structure that is considered to the Fe50Rh50 alloy mutually.
Fallot found for the first time to have the CsCl structure in 1938 orderly FeRh base alloy have one-level antiferromagnetic/ferromagnetic phase transition.Be heated to phase transition temperature (being approximately 350K) from room temperature, orderly FeRh alloy has experienced a magnetic phase transition from AFM to FM, and a magnetic lag (J.Lommel and J.Kouvel about 10K is arranged simultaneously; J.Appl.Phys.; Vol.38, pp1263～1264,1967).Discover that further the unit cell volume that is accompanied by 1%-2% in the phase transition process expands, reduction and a very big Entropy Changes of resistivity.In addition, at J.Appl.Phys., Vol.74, pp 3328,1993; J.Appl.Phys., Vol.90, pp6251,2001 and IEEE Tran.Magn., vol.40 has also studied the phase transformation of FeRh alloy in pp 2537,2004 documents such as grade.Utilize the antiferromagnetic/ferromagnetic first order phase change behavior of FeRh ordered alloy, J.Thiele etc. (pp 2537,2004 for IEEE Tran.Magn., vol.40) have developed the FeRh/FePt bilayer film that is used for HAMR; Zhou etc. (U.S. Pat 20090052092A1) have developed the perpendicular magnetic recording head that contains the FeRh layer; E.Fullerton etc. (U.S. Pat 007372116B2) have developed has the auxiliary magnetic that overturns of heat memory cell immediately.
Generally, the orderly FeRh alloy of CsCl structure antiferromagnetic/temperature of ferromagnetic phase transition is about 350K.But its phase transition temperature is very sensitive to the composition of sample, can regulate through mixing.Add a spot of Ir or Pt to improve phase transition temperature and add little P d and can reduce phase transition temperature.Through regulating the antiferromagnetic/ferromagnetic transition temperature of FeRh base alloy, exist so, can make this alloy have more broad range of techniques possibility of its application, such as HAMR medium, Spin Valve, magnetic refrigeration and micro-nano electro-mechanical system etc.
Summary of the invention
The objective of the invention is to overcome the defective of prior art; Regulate the antiferromagnetic/ferromagnetic transition temperature of alloy firm through the Pt that in the FeRh alloy firm, adds different amounts; Adjustable FeRhPt laminated film of a kind of phase transition temperature and preparation method thereof is provided, makes it satisfy the technical application on wider scope.
First aspect present invention discloses the adjustable FeRhPt laminated film of a kind of phase transition temperature, comprise monocrystalline MgO (001) substrate with and on (FeRh) 100-XPt XAlloy firm, and the span of x is 0<x<20.
More excellent, said (FeRh) 100-XPt XAlloy firm thickness is 5～100nm.
Second aspect present invention discloses the preparation method of the adjustable FeRhPt laminated film of aforementioned phase transition temperature, and step is:
1) depositing of thin film: on monocrystalline (001) MgO substrate, deposit (FeRh) through sedimentation 100-XPt XAlloy firm, wherein the span of x is 0<x<20;
2) annealing in process: behind the substrate natural cooling, the film that in a vacuum deposition is obtained carries out annealing in process and obtains the FeRhPt laminated film.
More excellent, said sedimentation is a physical vaporous deposition.
More excellent, said sedimentation is the magnetron sputtering deposition method.
Said magnetron sputtering deposition method is: adopt Fe 50Rh 50The method of alloy target material and Pt target cosputtering is carried out sputter in argon gas atmosphere.
Optimum, the condition of said magnetron sputtering deposition method is: 100～500 ℃ of sputter time substrate temperatures; Vacuum tightness 0.7 * 10 at the bottom of the back of the body of sputtering chamber -5～* 10 -5Pa, ar pressure 1～20Pa during sputter.
Optimum, substrate rotates with 5 rev/mins～30 rev/mins speed in the magnetron sputtering deposition method sputter procedure.
More excellent, the condition of said annealing in process is: vacuum tightness 1 * 10 -5～10 * 10 -5Pa, 400～700 ℃ of annealing temperatures, annealing time 0.5～4 hour.
Third aspect present invention discloses the application of the adjustable FeRhPt laminated film of aforementioned phase transition temperature as magnetic recording media.
The present invention adopts monocrystalline MgO (001) as substrate, mainly is for the epitaxial growth that realizes the FeRhPt film and vertical orientated, obtains comparatively perfectly CsCl ordered structure; Preparation method of the present invention in addition also brings out the ordering that the FeRhPt laminated film is accomplished through annealing in process; Has antiferromagnetic/ferromagnetic phase transition; Final obtain a series of antiferromagnetic/FeRhPt laminated film that ferromagnetic transition temperature is adjustable, make this alloy have more broad range of techniques possibility of its application.Preparation method of the present invention material property simple, preparation is good, and the utmost point is applicable to the preparation of the FeRhPt laminated film that phase transition temperature is adjustable.
Description of drawings
Fig. 1: the magnetization of FeRhPt laminated film and the graph of a relation of temperature
Fig. 2: X ray diffracting spectrum
Embodiment
Further set forth the present invention below in conjunction with specific embodiment, should be understood that embodiment only is used to the present invention is described and is not used in restriction protection scope of the present invention.
Embodiment 1
1. experimental technique
1) at first utilize ultrasonic cleaning equipment in alcoholic solution, to clean monocrystalline MgO (001) substrate, and dry up with pressurized air, the MgO substrate after with tweezers cleaning being dried up is placed on the sputtering chamber sample base.
2) treat the sputter back lining at the bottom of vacuum reach 2 * 10 -5Utilize radiofrequency magnetron sputtering technology on the MgO of cleaning substrate, to pass through co-sputtering technology during Pa, adopt Fe 50Rh 50The method of alloy target material and Pt target cosputtering, deposition (FeRh) 95Pt 5Alloy firm (numerical value in the chemical formula is mol ratio), its thickness is at 50nm.When sputter, substrate temperature is 100 ℃.Ar pressure is 10Pa during sputter.In sputter procedure, substrate rotates with 12 rev/mins speed.
3) after sputter finishes, substrate is naturally cooled to room temperature, put into the vacuum annealing furnace thermal treatment of annealing then.Vacuum tightness is 10 * 10 at the bottom of the back of the body of vacuum annealing furnace -5Pa, annealing temperature is 700 ℃, annealing time is 0.5 hour.
2. experimental result
Through detecting, the film of preparing is antiferromagnetic/and ferromagnetic transition temperature is about 450K, and Curie temperature is about 650K, (FeRh) 95Pt 5The relation curve of the laminated film magnetization and temperature is as shown in Figure 1.
Embodiment 2
1. experimental technique
1) at first utilizes ultrasonic cleaning equipment in alcoholic solution, to clean monocrystalline MgO (001) substrate, and dry up with pressurized air.MgO substrate after with tweezers cleaning being dried up is placed on the sputtering chamber sample base.
2) treat the sputter back lining at the bottom of vacuum reach 0.7 * 10 -5Utilize radiofrequency magnetron sputtering technology on the MgO of cleaning substrate, to pass through co-sputtering technology during Pa, adopt Fe 50Rh 50The method of alloy target material and Pt target cosputtering, deposition (FeRh) 90Pt 10Alloy firm (numerical value in the chemical formula is mol ratio), its thickness is at 100nm.When sputter, substrate temperature is 350 ℃.Ar pressure is 20Pa during sputter.In sputter procedure, substrate rotates with 5 rev/mins speed.
3) after sputter finishes, substrate is naturally cooled to room temperature, put into the vacuum annealing furnace thermal treatment of annealing then.Vacuum tightness is 5 * 10 at the bottom of the back of the body of vacuum annealing furnace -5Pa, annealing temperature is 500 ℃, annealing time is 2 hours.
2. experimental result
Through detecting, the film of preparing is antiferromagnetic/and ferromagnetic transition temperature is about 490K, and Curie temperature is about 600K.The relation curve of its magnetization and temperature is as shown in Figure 1.
Embodiment 3
1. experimental technique
1) at first utilizes ultrasonic cleaning equipment in alcoholic solution, to clean monocrystalline MgO (001) substrate, and dry up with pressurized air.MgO substrate after with tweezers cleaning being dried up is placed on the sputtering chamber sample base.
2) treat the sputter back lining at the bottom of vacuum reach 5 * 10 -5Utilize radiofrequency magnetron sputtering technology on the MgO of cleaning substrate, to pass through co-sputtering technology during Pa, adopt Fe 50Rh 50The method of alloy target material and Pt target cosputtering, deposition (FeRh) 85Pt 15Alloy firm (numerical value in the chemical formula is mol ratio), its thickness is at 5nm.When sputter, substrate temperature is 500 ℃.Ar pressure is 1.0Pa during sputter.In sputter procedure, substrate rotates with 30 rev/mins speed.
3) after sputter finishes, substrate is naturally cooled to room temperature, put into the vacuum annealing furnace thermal treatment of annealing then.Vacuum tightness is 1 * 10 at the bottom of the back of the body of vacuum annealing furnace -5Pa, annealing temperature is 400 ℃, annealing time is 4 hours.
2. experimental result
Through detecting, the film of preparing is antiferromagnetic/and ferromagnetic phase transition is about 520K, and Curie temperature is about 570K.The relation curve of its magnetization and temperature is as shown in Figure 1.
Can find out that from the graph of relation of the embodiment 1-3 material magnetization and temperature the FeRhPt film for preparing all has antiferromagnetic/ferromagnetic phase transition; Its phase transition temperature raises along with the increase of Pt content, and Curie temperature reduces along with the increase of Pt content, and the thermo-lag width that is accompanied by phase transformation increases along with Pt content and reduces.
X-ray diffraction shown in Figure 2 shows that film has the body-centered cubic structure of vertical orientated CsCl type; Show and utilize magnetically controlled sputter method to prepare the FeRhPt film; Again through subsequent heat treatment can obtain to have the CsCl ordered structure, the FeRhPt film of characteristics such as vertical orientated and phase transition temperature is adjustable, be applicable to the application of following HAMR medium, Spin Valve, magnetic refrigeration and micro-nano electro-mechanical system etc.
The above; Being merely preferred embodiment of the present invention, is not to any formal and substantial restriction of the present invention, should be understood that; For those skilled in the art; Under the prerequisite that does not break away from the inventive method, also can make some improvement and replenish, these improvement and replenish and also should be regarded as protection scope of the present invention.Allly be familiar with the professional and technical personnel, under the situation that does not break away from the spirit and scope of the present invention, the technology contents that is disclosed more than capable of using and a little change of making, modify the equivalent variations with differentiation, be equivalent embodiment of the present invention; Simultaneously, the change of any equivalent variations that all foundations essence technology of the present invention is done the foregoing description, modify and differentiation, all still belong in the scope of technical scheme of the present invention.

Claims (9)

1. FeRhPt laminated film that phase transition temperature is adjustable, comprise monocrystalline MgO (001) substrate with and on (FeRh) 100-XPt XAlloy firm, and the span of x is 0<x<20.
2. FeRhPt laminated film as claimed in claim 1 is characterized in that, said (FeRh) 100-XPt XAlloy firm thickness is 5～100nm.
3. the preparation method of claim 1 or 2 described FeRhPt laminated films, step is:
1) depositing of thin film: on monocrystalline (001) MgO substrate, deposit (FeRh) through sedimentation 100-XPt XAlloy firm, wherein the span of x is 0<x<20;
2) annealing in process: behind the substrate natural cooling, the film that in a vacuum deposition is obtained carries out annealing in process and obtains the FeRhPt laminated film.
4. preparation method as claimed in claim 3 is characterized in that, the said sedimentation of step 1) is a physical vaporous deposition.
5. preparation method as claimed in claim 4 is characterized in that, the said sedimentation of step 1) is the magnetron sputtering deposition method.
6. preparation method as claimed in claim 5 is characterized in that, the condition of said magnetron sputtering deposition method is: 100～500 ℃ of sputter time substrate temperatures; Vacuum tightness 0.7 * 10 at the bottom of the back of the body of sputtering chamber -5～5 * 10 -5Pa, ar pressure 1～20Pa during sputter.
7. preparation method as claimed in claim 5 is characterized in that, substrate rotates with 5 rev/mins～30 rev/mins speed in the magnetron sputtering deposition method sputter procedure.
8. preparation method as claimed in claim 3 is characterized in that step 2) condition of said annealing in process is: vacuum tightness 1 * 10 -5～10 * 10 -5Pa, 400～700 ℃ of annealing temperatures, annealing time 0.5～4 hour.
9. claim 1 or the described FeRhPt laminated film of 2 arbitrary claims are as the application of magnetic recording media.
CN201210251569.6A 2012-07-19 2012-07-19 FeRhPt laminated film that a kind of phase transition temperature is adjustable and preparation method thereof Expired - Fee Related CN102779533B (en)

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Cited By (7)

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Publication number Priority date Publication date Assignee Title
CN103440875A (en) * 2013-08-13 2013-12-11 同济大学 FeRh/FePt bi-layer film for super high density heat assisted magnetic recording and preparation method thereof
CN104318932A (en) * 2014-10-29 2015-01-28 西南大学 Magnetic storage medium film adjustable in phase-transition temperature and coercive force and manufacturing method thereof
CN105321573A (en) * 2014-07-31 2016-02-10 希捷科技有限公司 Data reader with tuned microstructure
CN110614378A (en) * 2019-08-21 2019-12-27 电子科技大学 Preparation method of iron rhodium alloy powder with first-order phase change characteristic and magnetocaloric effect
CN110870029A (en) * 2017-04-11 2020-03-06 国家科学研究中心 Method for obtaining materials with a huge magnetocaloric effect by ion irradiation
CN110867511A (en) * 2018-08-28 2020-03-06 中电海康集团有限公司 Perpendicular magnetized MTJ device
CN112614935A (en) * 2020-12-11 2021-04-06 杭州电子科技大学 Method for simulating artificial synapse based on resistance effect of first-order magnetic phase change material

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CN102061451A (en) * 2010-12-14 2011-05-18 吉林师范大学 Preparation method of L10-FePt granular film

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CN1317695C (en) * 2005-07-06 2007-05-23 北京科技大学 Method for improving L10-Fept thin film performance with surface activating agent
CN102061451A (en) * 2010-12-14 2011-05-18 吉林师范大学 Preparation method of L10-FePt granular film

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103440875A (en) * 2013-08-13 2013-12-11 同济大学 FeRh/FePt bi-layer film for super high density heat assisted magnetic recording and preparation method thereof
CN105321573A (en) * 2014-07-31 2016-02-10 希捷科技有限公司 Data reader with tuned microstructure
CN104318932A (en) * 2014-10-29 2015-01-28 西南大学 Magnetic storage medium film adjustable in phase-transition temperature and coercive force and manufacturing method thereof
CN110870029A (en) * 2017-04-11 2020-03-06 国家科学研究中心 Method for obtaining materials with a huge magnetocaloric effect by ion irradiation
CN110867511A (en) * 2018-08-28 2020-03-06 中电海康集团有限公司 Perpendicular magnetized MTJ device
CN110867511B (en) * 2018-08-28 2021-09-21 中电海康集团有限公司 Perpendicular magnetized MTJ device
CN110614378A (en) * 2019-08-21 2019-12-27 电子科技大学 Preparation method of iron rhodium alloy powder with first-order phase change characteristic and magnetocaloric effect
CN110614378B (en) * 2019-08-21 2021-12-03 电子科技大学 Preparation method of iron rhodium alloy powder with first-order phase change characteristic and magnetocaloric effect
CN112614935A (en) * 2020-12-11 2021-04-06 杭州电子科技大学 Method for simulating artificial synapse based on resistance effect of first-order magnetic phase change material
CN112614935B (en) * 2020-12-11 2023-05-26 杭州电子科技大学 Method for simulating artificial synapse based on resistance effect of primary magnetic phase change material

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