CN102061451A - Preparation method of L10-FePt granular film - Google Patents
Preparation method of L10-FePt granular film Download PDFInfo
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- CN102061451A CN102061451A CN 201010585896 CN201010585896A CN102061451A CN 102061451 A CN102061451 A CN 102061451A CN 201010585896 CN201010585896 CN 201010585896 CN 201010585896 A CN201010585896 A CN 201010585896A CN 102061451 A CN102061451 A CN 102061451A
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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 L1 of high (001) degree of order of magnetic field preannealing preparation
0The method of-FePt particle film.
Background technology
Has L1
0The FePt film of ordered structure has high magnetocrystalline anisotropy, big coercive force, big saturation magnetization, high Curie temperature and good chemical stability and causes extensive concern both domestic and external, becomes the research focus of novel magnetic storage medium.L1
0-FePt particle film has good comprehensive performances, can satisfy the needs of super-high density magnetic recording to 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, the L1 of orderly center of area four directions (fct) structure of heated substrate depositing operation or subsequent heat treatment prepared generally adopted
0-FePt film.Which kind of technology no matter, difficulty that is faced 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
0-FePt particulate height (001) preferred orientation and excellent magnetism energy.At 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: as interfacial layer, top layer, bottom; 2) select suitable substrate material; 3) improve preparation technology: 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 significant effects to the microtexture of magneticsubstance.Magnetic-field annealing is handled can be reduced transformation temperature to a certain extent, promotes texture growing and improve magnetic property, all selects the FePt film is carried out magnetic-field annealing but have research now, does not bring out L1 effectively
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 suitable extensive studies, but still need carry out number of research projects 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, this method is realized by following steps:
Step 1, at room temperature adopts direct current magnetron sputtering process to prepare the FeAg nano thin-film on substrate;
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 not have the magnetic field vacuum annealing after FeAg nano thin-film after the annealing at room temperature adopts magnetically controlled DC sputtering deposition Pt layer, obtain L1
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 prepares single-phase (fcc) structure FeAg super saturated solid solution body thin film by adopting magnetically controlled sputter method, and magnetic-field annealing prepares pre-texture Fe (001)/Ag film, explore the micromechanism that film is separated, realize the texture and the microstructure control of α-Fe crystal grain.On α-Fe (Ag) film that obtains Fe (001) texture growing, deposit Pt, 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, reduce the ordering temperature of FePt effectively, formed the high-performance L1 high degree of order, little grain-size, that the intercrystalline magnetic interaction is little on the substrate arbitrarily
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 at the FePt/Ag film that obtains of the present invention on the FeAg film basis of 400 ℃ zero magnetic field preannealings;
Fig. 2 is the magnetic hysteresis loop of the FePt/Ag film that obtains on the FeAg film basis of preannealing of the present invention through 400 ℃ and magnetic field 10kOe the time.
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, this method is realized by following steps:
Step 1, at room temperature adopts direct current magnetron sputtering process to prepare the FeAg nano thin-film on substrate;
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 not have the magnetic field vacuum annealing after FeAg nano thin-film after the annealing at room temperature adopts magnetically controlled DC sputtering deposition 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 0～10kOe magnetic field.
The described acquisition of step 3 L1 in the present embodiment
0The detailed process of-FePt film is: adopt magnetically controlled DC sputtering deposition Pt layer, obtain the Pt/FeAg film; Described Pt/FeAg film is not had the magnetic field vacuum annealing, finally obtain L1
0-FePt/Ag film.
The temperature of not having magnetic-field annealing in the present embodiment behind the described employing magnetically controlled DC sputtering deposition of the step 3 Pt layer 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 10kOe magnetic field pretreatment sample, when the subsequent anneal temperature was 400 ℃, its parallel face was respectively 7.43kOe and 5.38kOe 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 the transition temperature of unordered fcc to orderly fct structure FePt effectively, 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 handled: the described substrate of present embodiment is Si (a 001) substrate, and described substrate is cleaned 15min in acetone, ethanol and deionized water for ultrasonic, sends 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 the direct current cosputtering, the base vacuum of sputtering system is better than 1.5 * 10
-4Pa, the Ar operating air pressure is 4.5mTorr during sputter, and the substrate speed of rotation is 20r/min, and the purity of Fe and Ag target is 99.95%, obtains the FeAg nano thin-film;
Three, anneal: with the FeAg film sample that obtains in vacuum magnetic anneal stove respectively 0 and 10kOe magnetic field under carry out 400 ℃ of annealing, field direction obtains the FeAg film of Fe (001) texture growing perpendicular to face.
Four, choose through 0 magnetic field and 10kOe magnetic field when 400 ℃ of temperature and carry out preannealing FeAg film, room temperature d.c. sputtering deposition Pt layer obtains the Pt/FeAg film then.
Again the Pt/FeAg film is carried out handling 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 than obtaining the high degree of order, little grain-size, the mutual isolated L1 of intercrystalline under the low temperature thermal oxidation
0-FePt/Ag film.
The present invention adopts X-ray diffractometer and vibrating sample magnetometer that structures of samples and magnetic that present embodiment obtains are 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 facilitation, 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 (5)
1. L1
0The preparation method of-FePt particle film is characterized in that, this method is realized by following steps:
Step 1, at room temperature adopts direct current magnetron sputtering process to prepare the FeAg nano thin-film on substrate;
Step 2, the FeAg nano thin-film that step 1 is prepared place magnetic field to carry out vacuum annealing; FeAg nano thin-film after obtaining to anneal;
Step 3, step 2 is obtained not have the magnetic field vacuum annealing after FeAg nano thin-film after the annealing at room temperature adopts magnetically controlled DC sputtering deposition Pt layer, obtain L1
0-FePt/Ag film.
2. a kind of L1 according to claim 1
0The preparation method of-FePt particle film is characterized in that, 300～400 ℃ of the temperature of step 2 described magnetic field vacuum annealing, and annealing time is 0.5～1 hour.
3. a kind of L1 according to claim 1 and 2
0The preparation method of-FePt particle film is characterized in that, step 2 is described to place magnetic field to carry out vacuum annealing the FeAg nano thin-film, and described magnetic field is 0～10kOe magnetic field.
4. a kind of L1 according to claim 1
0The preparation method of-FePt particle film is characterized in that, the described acquisition of step 3 L1
0The detailed process of-FePt/Ag film is: adopt magnetically controlled DC sputtering deposition Pt layer, obtain the Pt/FeAg film; Described Pt/FeAg film is not had the magnetic field vacuum annealing, finally obtain L1
0-FePt/Ag film.
5. according to claim 1 or 4 described a kind of L1
0The preparation method of-FePt particle film is characterized in that, the temperature of not having the magnetic field vacuum annealing behind the described employing magnetically controlled DC sputtering deposition of the step 3 Pt layer is 300～600 ℃, and annealing time is 0.5～1 hour.
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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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|---|---|---|---|
| CN 201010585896 CN102061451B (en) | 2010-12-14 | 2010-12-14 | Preparation method of L10-FePt granular film |
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| CN102061451A true CN102061451A (en) | 2011-05-18 |
| CN102061451B CN102061451B (en) | 2013-01-02 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102779533A (en) * | 2012-07-19 | 2012-11-14 | 同济大学 | FeRhPt composite film adjustable in phase transition temperature and preparation method of FeRhPt composite film |
| CN103065646A (en) * | 2011-10-24 | 2013-04-24 | 南通海纳电子纳米科技有限公司 | FePt nanometer cluster magnetic recording media |
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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Patent 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 |
Non-Patent Citations (1)
| Title |
|---|
| 《电子元件与材料》 20100131 赵书华，等 "磁场退火对FePt/Ag薄膜磁性能的影响" 33-34 1-5 第29卷, 第1期 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103065646A (en) * | 2011-10-24 | 2013-04-24 | 南通海纳电子纳米科技有限公司 | FePt nanometer cluster magnetic recording media |
| 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 |
| CN102779533A (en) * | 2012-07-19 | 2012-11-14 | 同济大学 | FeRhPt composite film adjustable in phase transition temperature and preparation method of FeRhPt composite film |
| 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 |
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