CN102061451B - Preparation method of L10-FePt granular film - Google Patents
Preparation method of L10-FePt granular film Download PDFInfo
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- CN102061451B CN102061451B CN 201010585896 CN201010585896A CN102061451B CN 102061451 B CN102061451 B CN 102061451B CN 201010585896 CN201010585896 CN 201010585896 CN 201010585896 A CN201010585896 A CN 201010585896A CN 102061451 B CN102061451 B CN 102061451B
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Abstract
The invention discloses a preparation method of an L10-FePt granular film, relating to a method for preparing an L10-FePt granular film with high degree of order by preannealing in a magnetic field, which has the advantages of lowering the ordering temperature of a FePt granular film, promoting the growth of tissues of the L10-FePt granular film (001) and improving the magnetic property and comprises the following steps of: firstly, preparing a FeAg nano film on a substrate at room temperature by using a DC magnetic control sputtering method; secondly, placing the FeAg nano film prepared in the first step into the magnetic field and carrying out vacuum annealing to obtain an annealed FeAg nano film; and thirdly, depositing the annealed FeAg nano film obtained in the second step at room temperature by DC magnetic control sputtering to form a Pt layer, and then carrying out vacuum annealing without any magnetic field to obtain the L10-FePt/Ag film. With the method provided by the invention, the high-performance L10-FePt/Ag film with high degree of order, small crystallite size and small magnetic mutual effects among crystalline grains can be formed on any substrate.
Description
Technical field
The present invention relates to utilize the magnetic field preannealing to prepare the L1 of high (001) degree of order
0The method of-FePt particle film.
Background technology
Has L1
0The FePt film of ordered structure has high magnetocrystalline anisotropy, large coercive force, large saturation magnetization, high Curie temperature and good chemical stability and causes extensive concern both domestic and external, becomes the study hotspot of New Magnetic Field Controlled storage media.L1
0-FePt particle film has good over-all properties, can satisfy the super-high density magnetic recording to the needs of thermostability, is considered to the most promising magnetic recording material.
Utilize the FePt film of sedimentation room temperature preparation to be generally unordered face-centered cubic (fcc) structure, so, generally adopt heated substrate depositing operation or subsequent heat treatment technique to prepare the L1 of orderly center of area four directions (fct) structure
0-FePt film.Which kind of technique no matter, the difficulty that faces and the problem that does not solve fully are: how on the basis that reduces ordering temperature, keep less L1
0-FePt crystal grain is realized L1
0The height of-FePt particle (001) preferred orientation and excellent magnetic property.For this key problem, people have carried out broad research, have obtained many valuable results of study.
The ordering temperature that how to reduce the FePt film is one of the most active problem of this field Recent study.People have adopted multiple means to attempt reducing its ordering temperature: 1) add element: such as interfacial layer, top layer, bottom; 2) select suitable substrate material; 3) improve preparation technology: such as ion irradiation method and plasma method etc.; 4) impressed pressure or magnetic field; 5) FePt multilayer film or alternating deposit etc.
Aspect thermomagnetic treatment, it is found that, thermomagnetic treatment has important impact to the microtexture of magneticsubstance.Magnetic-field annealing is processed can be reduced to a certain extent transformation temperature, promotes texture growing and improve magnetic property, all selects the FePt film is carried out magnetic-field annealing but have research now, does not effectively bring out L1
0(001) texture of-FePt film, this mainly is because the saturation magnetization (Ms) of FePt film is less, and Zeeman can be lower, therefore the effect in magnetic field is reduced.
Although should be pointed out that people are about L1
0-FePt film has carried out quite widely research, but still need carry out a large amount of research work at aspects such as texture control, organization optimizations.
Summary of the invention
Ordering temperature, the promotion L1 of the present invention for reducing the FePt film
0(001) texture growing of-FePt film, improve its magnetic property, a kind of L1 is provided
0The preparation method of-FePt particle film.
A kind of L1
0The preparation method of-FePt particle film, the method is realized by following steps:
Step 1, at room temperature adopts direct current magnetron sputtering process at substrate preparation supersaturated solid solution FeAg nano thin-film;
Step 2, the supersaturated solid solution FeAg nano thin-film that step 1 is prepared place magnetic field to carry out vacuum annealing; Pre-texture Fe (001) after obtaining to anneal/Ag film; The temperature of magnetic field vacuum annealing is 300 ~ 400 ℃, and annealing time is 0.5 ~ 1 hour, and magneticstrength is 10 kOe;
Step 3, the pre-texture Fe (001)/Ag film that step 2 is obtained after the annealing carry out without the magnetic field vacuum annealing after at room temperature adopting Deposited By Dc Magnetron Sputtering Pt layer, obtain L1
0-FePt/Ag film;
Described acquisition L1
0The detailed process of-FePt/Ag film is: adopt magnetically controlled DC sputtering at pre-texture Fe (001)/Ag film deposition Pt layer, obtain the Pt/FeAg film; Described Pt/FeAg film is carried out finally obtaining L1 without the magnetic field vacuum annealing
0-FePt/Ag film.
Principle of the present invention: the present invention adopts magnetron sputtering method to prepare the FeAg nano thin-film, in magnetic field the FeAg film is annealed, and behind magnetron sputtering deposition Pt on the FeAg film of pre-texture, carries out non-magnetic field annealing.The present invention is by adopting magnetically controlled sputter method to prepare single-phase (fcc) structure FeAg super saturated solid solution body thin film, and magnetic-field annealing prepares pre-texture Fe (001)/Ag film, explore the micromechanism that film is separated, realize texture and the microstructure control of α-Fe crystal grain.Deposit Pt at α-Fe (Ag) film that obtains Fe (001) texture growing, pass through L1
0The dynamic (dynamical) research of the research of-FePt growth mechanism and ordering prepares the L1 of the high degree of order
0-FePt particle film.
Beneficial effect of the present invention: the present invention adopts magnetron sputtering method to prepare phase structure FeAg super saturated solid solution body thin film, prepare pre-texture Fe (001)/Ag film by magnetic-field annealing, effectively reduced the ordering temperature of FePt, at the high-performance L1 that substrate formation is the high degree of order, little grain-size arbitrarily, the intercrystalline magnetic interaction is little
0-FePt film.The present invention is significant for the acquisition of super-high density magnetic recording material.
Description of drawings
Fig. 1 is the magnetic hysteresis loop of the FePt/Ag film that obtains at the FeAg Membranous Foundations through 400 ℃ of zero magnetic field preannealings of the present invention;
Fig. 2 is the magnetic hysteresis loop of the FePt/Ag film that the FeAg Membranous Foundations of preannealing obtains through 400 ℃ and magnetic field 10 kOe time the of the present invention.
Embodiment
Embodiment one, in conjunction with Fig. 1 and Fig. 2 present embodiment is described, a kind of L1
0The preparation method of-FePt particle film, the method is realized by following steps:
Step 1, at room temperature adopts direct current magnetron sputtering process at substrate preparation FeAg nano thin-film;
Step 2, the FeAg nano thin-film that step 1 is prepared place magnetic field to carry out vacuum annealing, the FeAg nano thin-film after obtaining to anneal;
Step 3, step 2 is obtained to carry out without the magnetic field vacuum annealing after FeAg nano thin-film after the annealing at room temperature adopts Deposited By Dc Magnetron Sputtering Pt layer, obtain L1
0-FePt/Ag film.
300 ~ 400 ℃ of the temperature of step 2 described magnetic field vacuum annealing in the present embodiment, annealing time are 0.5 ~ 1 hour; Described magneticstrength is 0 ~ 10 kOe magnetic field.
The described acquisition of step 3 L1 in the present embodiment
0The detailed process of-FePt film is: adopt Deposited By Dc Magnetron Sputtering Pt layer, obtain the Pt/FeAg film; Described Pt/FeAg film is carried out finally obtaining L1 without the magnetic field vacuum annealing
0-FePt/Ag film.
The temperature of carrying out without magnetic-field annealing behind the described employing Deposited By Dc Magnetron Sputtering of the step 3 Pt layer in the present embodiment is 300 ~ 600 ℃, and annealing time is 0.5 ~ 1 hour.
Provided the result that the invention process is listed as in conjunction with Fig. 1 and Fig. 2.As seen from Figure 1, for zero magnetic field pretreatment sample, when the subsequent anneal temperature was 400 ℃, the coercive force of sample was less, presents soft magnetic property, did not also form Hard Magnetic phase L1 in the interpret sample
0-FePt; As seen from Figure 2, for 10 kOe magnetic field pretreatment sample, when the subsequent anneal temperature was 400 ℃, its parallel face was respectively 7.43 kOe and 5.38 kOe with vertical face coercive force, presents the Hard Magnetic characteristic, has formed Hard Magnetic phase L1 in the interpret sample
0-FePt.Fig. 2 shows, compares with the zero pretreated sample in magnetic field, and the magnetic-field annealing pre-treatment has reduced unordered fcc effectively to the transition temperature of orderly fct structure FePt, at 400 ℃ of L1 that can obtain high-coercive force
0-FePt film.
Embodiment two, present embodiment are embodiment one described a kind of L1
0The preparation method's of-FePt particle film specific embodiment:
One, substrate is processed: the described substrate of present embodiment is Si(001) substrate, described substrate is cleaned 15 min in acetone, ethanol and deionized water for ultrasonic, send into vacuum chamber after the drying;
Two, mode of deposition: at room temperature, adopt ATC 1800-F type multi-target magnetic control sputtering system to adopt dc sputturing method, the base vacuum of sputtering system is better than 1.5 * 10
-4Pa, the Ar operating air pressure is 4.5 mTorr during sputter, and the substrate speed of rotation is 20 r/min, and the purity of Fe and Ag target is 99.95%, obtains the FeAg nano thin-film;
Three, anneal: the FeAg film sample that obtains is carried out respectively 400 ℃ of annealing under 0 and 10 kOe magnetic fields in the Vacuum Magnetic annealing furnace, field direction obtains Fe(001 perpendicular to face) the FeAg film of texture growing.
Four, choose through 0 magnetic field and 10 kOe magnetic fields when 400 ℃ of temperature and carry out preannealing FeAg film, then room temperature d.c. sputtering deposition Pt layer obtains the Pt/FeAg film.
Again the Pt/FeAg film is carried out processing in magnetic-field annealing through differing temps under zero magnetic field, obtain the FePt/Ag film; Described different magnetic-field annealing temperature can be 300 ℃, 400 ℃, 500 ℃, 600 ℃;
Five, finally at the L1 high degree of order, little grain-size than acquisition under the low temperature thermal oxidation, that intercrystalline is isolated mutually
0– FePt/Ag film.
The present invention adopts X-ray diffractometer and vibrating sample magnetometer that the structure and magnetic property of the sample of the present embodiment acquisition is analyzed, the result shows, annealing FeAg film in magnetic field, the reduction of FePt/Ag film ordering temperature and the raising of magnetic there is obvious promoter action, compare with zero magnetic field pretreatment sample, the FePt/Ag film sample that obtains through the magnetic field pre-treatment can form L1 in 400 ℃ of annealing
0– FePt phase, the ordering temperature of FePt obviously reduces, and the degree of order and the coercive force of sample obviously increase.
Claims (1)
1. L1
0The preparation method of-FePt particle film is characterized in that, the method is realized by following steps:
Step 1, at room temperature adopts direct current magnetron sputtering process at substrate preparation supersaturated solid solution FeAg nano thin-film;
Step 2, the supersaturated solid solution FeAg nano thin-film that step 1 is prepared place magnetic field to carry out vacuum annealing; Pre-texture Fe (001) after obtaining to anneal/Ag film; The temperature of magnetic field vacuum annealing is 300 ~ 400 ℃, and annealing time is 0.5 ~ 1 hour, and magneticstrength is 10 kOe;
Step 3, the pre-texture Fe (001)/Ag film that step 2 is obtained after the annealing carry out without the magnetic field vacuum annealing after at room temperature adopting Deposited By Dc Magnetron Sputtering Pt layer, obtain L1
0-FePt/Ag film;
Described acquisition L1
0The detailed process of-FePt/Ag film is: adopt magnetically controlled DC sputtering at pre-texture Fe (001)/Ag film deposition Pt layer, obtain the Pt/FeAg film; Described Pt/FeAg film is carried out finally obtaining L1 without the magnetic field vacuum annealing
0-FePt/Ag film.
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| CN 201010585896 CN102061451B (en) | 2010-12-14 | 2010-12-14 | Preparation method of L10-FePt granular film |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010585896 CN102061451B (en) | 2010-12-14 | 2010-12-14 | Preparation method of L10-FePt granular film |
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| CN102061451B true CN102061451B (en) | 2013-01-02 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103065646B (en) * | 2011-10-24 | 2014-12-10 | 江苏海纳纳米技术开发有限公司 | FePt nanometer cluster magnetic recording media |
| CN102779533B (en) * | 2012-07-19 | 2016-04-06 | 同济大学 | FeRhPt laminated film that a kind of phase transition temperature is adjustable and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1822114A (en) * | 2006-03-10 | 2006-08-23 | 北京科技大学 | Method for preparing FePt/Ag high density magnetic recording medium material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1822114A (en) * | 2006-03-10 | 2006-08-23 | 北京科技大学 | Method for preparing FePt/Ag high density magnetic recording medium material |
Non-Patent Citations (2)
| Title |
|---|
| 赵书华，等."磁场退火对FePt/Ag薄膜磁性能的影响".《电子元件与材料》.2010,第29卷(第1期),33-34. |
| 赵书华,等."磁场退火对FePt/Ag薄膜磁性能的影响".《电子元件与材料》.2010,第29卷(第1期),33-34. * |
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