CN102864424B - Preparation method of magnetic recording film - Google Patents
Preparation method of magnetic recording film Download PDFInfo
- Publication number
- CN102864424B CN102864424B CN201210382689.XA CN201210382689A CN102864424B CN 102864424 B CN102864424 B CN 102864424B CN 201210382689 A CN201210382689 A CN 201210382689A CN 102864424 B CN102864424 B CN 102864424B
- Authority
- CN
- China
- Prior art keywords
- film
- mgo
- fept
- atom
- sputtering
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Abstract
The invention relates to a preparation method of L10-phase FePt-MgO magnetic recording film which is vertically aligned and small in grain size. The preparation method includes: firstly, cleaning a substrate the surface of which is provided with a silicon oxide layer; secondly, growing a FePt-MgO film on the surface of the substrate by vacuum co-sputtering; and thirdly annealing the film under vacuum, wherein the ratio of Fe atoms to Pt atoms in the film is 31:69-51:49, the volume ratio of MgO to the film is 5%-40%, Fe is sputtered by means of direct-current sputtering, and Pt and MgO are sputtered by alternating-current sputtering.
Description
Technical field
[0001] the present invention relates to a kind of preparation method of magnetic recording material, particularly a kind of have little grain-size, vertical orientated,
l1
0the material preparation method that contains Fe and Pt of phase.
Background technology
Along with the development of social progress, science and technology, people rapidly increase for the demand of information.The information of covering the sky and the earth and coming, has brought great challenge to the hard-disk capacity of its storage.In Future Society, economy and development in science and technology new focus is by the development that is Internet of Things, and this will make quantity of information sharply expand.At present, mainly contain three kinds of information storage modes: (1) magnetic stores, as floppy disk and hard disk, tape etc.; (2) electricity stores, as solid state hard disc, and semiconductor flash memory etc.; (3) light stores, as CD CD and DVD CD etc.In the mode of so many storage, magnetic stores and occupies great advantage: as cost is low, recording density is high, good stability etc.So, to compare with optical storage with semiconductor storage, magnetic saves as the major way of current information storage, almost in occupation of more than 90% storage market.And hard disc data recording areal density increases with the rate of growth of annual 30 %-40 %, 2005, whole world storage informational capacity was less than 900 PB(PB=1X10
15byte), and be increased to 7000 PB during by 2010,5 years increased nearly 8 times.What return to zero mainly adopted now is spin-exchange-coupled combined-type magnetic recording technique, and within 2010, this technology has made area recording density break through 800 Gb/in
2.Next adopt spin-exchange-coupled Magnetographic Technology to make area recording density surpass 2 Tb/in continuation
2.As can be seen here, in following decades, magnetic recording still occupies irreplaceable status in Computer Storage field.
In order to increase magnetic storage density, the particle that records in the perpendicular magnetic recording medium adopting at present must be enough little, and particle size reduce to cause superparamagnetic effect, so must use
l1
0this high magnetocrystalline anisotropy energy (6 ~ 10X10 of FePt ordered alloy
7erg/cc) material improves thermostability.The general particle size of FePt film for preparing by magnetron sputtering method is at present larger or be continuous film, this large particle is clearly unfavorable for improving recording density, in continuous film, between FePt particle, there is very strong exchange-coupling interaction, can bring very large signal to noise ratio.So research preparation particle size smaller, vertical orientated
l1
0fePt film becomes the important topic in current magnetic recording field.
According to existing document, preparation particle size smaller, exchange-coupling interaction is more weak between particle
l1
0fePt film can obtain by ion beam irradiation, electron beam irradiation.But preparation is more time-consuming so in large area in magnetic recording application, moreover cost is also expensive.Another kind method is in FePt film, to mix oxide compound to carry out refinement and separate FePt particle, such as: Al
2o
3, MgO, SiO
2, TiO
2deng, at FePt-Al
2o
3in film, Al
2o
3although interpolation reduced to a certain extent FePt particle size, the degree of order of FePt film reduces greatly, and is unfavorable for that the easy magnetizing axis of film is vertical orientated.In the document of the doped with Mg O of report, there are people alternating sputtering FePt and MgO on different substrates at present, also have people cosputtering FePt and MgO on different substrates.During sputter substrate, generally all will heat, moreover particle size is all larger.Add SiO
2after, in order to form well
l1
0phase structure, must carry out rapid thermal process, temperature rise rate 100
oc/s, this just requires equipment for Heating Processing will have very high vacuum tightness, very high to equipment requirements.Adding TiO
2bibliographical information in, although FePt granular size is smaller, granule boundary is fuzzyyer, moreover preparation process is numerous and diverse.Above-mentioned these preparation methods, ubiquitous problem is that preparation process is complicated, and technical requirements is high, and difficulty is large.
Chinese invention patent 200710173302.9 and 200610118917.7 discloses respectively vertical orientated
l1
0the preparation method of phase FePt magnetic recording thin film.In these two patents, all need between substrate and FePt layer, add substrate layer, its preparation process is comparatively complicated; Secondly, the granular size of the uncontrollable film preparing in these two patents, oarse-grainedly in the particle of estimating to prepare by this patent will account for very large advantage.
Summary of the invention
The invention provides a kind of prior art deficiency that overcomes, can prepare and there is the very method of small-particle and the anisotropic magnetic recording particles film of good vertical.
Of the present invention have a little grain-size and vertical orientated
l1
0first the preparation method of phase FePt-MgO magnetic recording thin film has the substrate of one deck silicon oxide through clean by its surface, then by vacuum cosputtering mode, at substrate surface cosputtering, grow one deck FePt-MgO film, wherein: in film, the ratio of Fe atom and Pt atom is 31:69-51:49, the volume ratio of MgO and film is 5%-40%; Sputter Fe is d.c. sputtering mode, and sputter Pt for exchanging sputter mode, and then carries out anneal by film with MgO under vacuum condition.
Little grain-size of the present invention and vertical orientated
l1
0in the preparation method of phase FePt-MgO magnetic recording thin film, in prepared film, the ratio of Fe atom and Pt atom is 47:53, and the volume ratio of MgO and film is 20%; In preparation process, the annealing temperature of film is 700 ℃.
Little grain-size of the present invention and vertical orientated
l1
0in the preparation method of phase FePt-MgO magnetic recording thin film, the vacuum tightness of sputtering chamber is less than 1.7X10
-7after Torr, start sputter and prepare film, sputtering pressure is 5 mTorr, difference build-up of luminance Fe target, Pt target and MgO target, and by adjusting the sputtering power of Fe target and Pt target, the ratio of Fe atom and Pt atom in control film, magnesian content is also controlled by controlling sputter rate, and magnesian sputtering power scope is 35w-240 w, and wherein best sputtering power is 95W; The FePt-MgO film preparing is annealed in vacuum annealing furnace, and in stove, vacuum tightness is less than 1X10
-3torr, annealing temperature is 700
oc, heating mode is for first rising to 50 from room temperature
oc, then 50
oc insulation 5 minutes, temperature rise rate is 50 thereafter
oc/min, annealing time is 60 minutes, heating finishes the rear temperature vacuum annealing furnace and is made as 0
oc, furnace chamber temperature drops to lower than 55 by the time
oafter C, take out film.
The present invention is a kind of growth technique of p-nJie Erjiguan non-epitaxial p-n junction diode formula, by Fe, Pt, MgO cosputtering, pyroprocessing then, can prepare easily particle size smaller, perpendicular magnetic anisotropy is reasonable
l1
0fePt particle film.Experiment shows, by the present invention, is prepared
l1
0phase FePt-MgO particle film has good orientation, good perpendicular magnetic anisotropy, the vertical direction coercive force of film has reached 12.5 kOe, rectangular degree close to 1, FePt even particle distribution, size close to 5 nm.
Accompanying drawing explanation
Fig. 1: the Si-SiO being prepared by the present invention
2the XRD diffraction spectra of/FePt (10 nm)-MgO (x vol.%).Wherein, be respectively that MgO volume fraction is respectively 5 % from top to bottom, 10 %, 15 %, 20 %, 25 %, 30 %, 35 %, the XRD diffraction spectra of the FePt-MgO particle film of 40 %.
Fig. 2: the Si-SiO being prepared by the present invention
2the magnetic hysteresis loop of/FePt (10 nm)-MgO (x vol.%).Wherein, (a) and (b), (c), (d), (e), (f) are respectively that MgO volume fraction is respectively 5 %, 10 %, 15 %, 20 %, 25 %, the magnetic hysteresis loop of the FePt-MgO particle film of 30 %.
Fig. 3: the Si-SiO being prepared by the present invention
2the transmission electron microscope picture of/FePt (10 nm)-MgO (20 vol.%)
Embodiment
The invention is further illustrated by the following examples,
Concrete steps of the present invention are as follows:
The thermooxidizing silicon chip that business is bought is put into acetone soln as substrate, with Ultrasonic Cleaners, cleans 10 min; Ultrasonic cleaning 10 min in raw spirit again.The F.F. sample chamber of cleaned substrate being put into vacuum sputtering coating device, vacuumizes; Vacuum tightness Deng F.F. sample chamber is less than 1.0X10
-5below Torr, substrate is sent and is delivered to sputtering chamber.Vacuum tightness Deng sputtering chamber is less than 1.7X10
-7after Torr, start to prepare film.First regulate the off-gas pump of sputtering chamber, then open rotary knob and make substrate rotation, again the argon gas of working gas is passed in chamber, the sputtering pressure of setting working gas is 5 mTorr, Deng sputtering pressure stable after, difference build-up of luminance Fe target, Pt target and MgO target, adjust the sputtering power of Fe target and Pt target, make in film after the ratio of Fe atom and Pt atom is determined value Inversion, adjust the sputtering power of MgO, make the content of MgO meet volume fraction required in FePt-MgO film, the content of MgO in FePt-MgO film by formula [
t mgO/ (
t fePt(10 nm)+
t mgO)] * 100 vol. % decisions, t is thickness, it is 0 %-40 % that MgO content accounts for FePt-MgO volume.。Then simultaneously with mode sputter Fe, Pt, the MgO of cosputtering, wherein sputter Fe is d.c. sputtering mode, sputter Pt with MgO for exchanging sputter mode.The sputtering power of Fe is 26 W, and sputter rate is 15.5/min; The sputtering power of Pt is 30 W, and sputter rate is 13/min; MgO is composite target material and volume content while being 20%, and sputtering power is 95 W, and sputter rate is 7/min.
Finally, the FePt-MgO film preparing is annealed in vacuum annealing furnace, in stove, vacuum tightness is less than 1X10
-3torr, annealing temperature is 700
oc, heating mode is for first rising to 50 from room temperature
oc, then 50
oc insulation 5 minutes, temperature rise rate is 50 thereafter
oc/min, annealing time is 60 minutes.Heating finishes the rear temperature vacuum annealing furnace and is made as 0
oc, furnace chamber temperature drops to lower than 55 by the time
oafter C, take out film.
Embodiment Si-SiO
2/ FePt (10 nm)-MgO (x vol.%) (x=0-40)
The CMS-18 multifunctional magnetic control sputtering equipment computerizeing control is prepared Si-SiO
2/ FePt (10 nm)-MgO (x vol.%) (x=0-40) magneticthin film.Using thermooxidizing silicon chip as substrate, after the good FePt-MgO of sputter, 700
oc anneals 60 minutes in vacuum annealing furnace, obtain needed film, its FePt atomic ratio is respectively 47:53, as shown in Figure 1, respectively that MgO volume fraction is respectively 5 % from top to bottom, 10 %, 15 %, 20 %, 25 %, 30 %, 35 %, the XRD diffraction spectra of the FePt-MgO particle film of 40 % can only be seen and take FePt(001 when MgO content is 5%-25%) and (002) peak be main crystalline orientation, the prepared FePt-MgO particle film that shows clearly has good orientation when MgO content is 5%-25%; When MgO content is 5%-30%, the magnetic hysteresis loop of sample, is shown in Fig. 2, wherein, (a) and (b), (c), (d), (e), (f) are respectively that MgO volume fraction is respectively 5 %, 10 %, 15 %, 20 %, 25 %, the magnetic hysteresis loop of the FePt-MgO particle film of 30 %.When MgO content is 20%, the transmission electron microscope picture of sample is shown in accompanying drawing 3, and as seen from the figure, when MgO content is 20%, the size distribution of prepared FePt-MgO film is more even, and particle size is close to 5 nm.Visible when MgO content is 20%, prepared FePt particle film has important using value in magnetic recording media.
Claims (3)
1. a preparation method for magnetic recording thin film, is characterized in that:
A. first there is to the substrate of one deck silicon oxide on its surface through clean, then by vacuum cosputtering mode, at substrate surface cosputtering, grow one deck FePt-MgO film, wherein: in film, the atomic ratio of Fe atom and Pt atom is 31:69-51:49, the volume ratio of MgO and film is 5%-40%; Sputter Fe is d.c. sputtering mode, and sputter Pt for exchanging sputter mode, and then carries out anneal by film with MgO under vacuum condition;
B. the vacuum tightness of sputtering chamber is less than 1.7X10
-7after Torr, start sputter and prepare film, sputtering pressure is 5 mTorr, difference build-up of luminance Fe target, Pt target and MgO target, and by adjusting the sputtering power of Fe target and Pt target, the ratio of Fe atom and Pt atom in control film, magnesian content is also to control by controlling sputter rate, and sputtering power scope is 35W-240W; The FePt-MgO film preparing is annealed in vacuum annealing furnace, and in stove, vacuum tightness is less than 1X10
-3torr, annealing temperature is 700
oc, heating mode is for first rising to 50 from room temperature
oc, then 50
oc insulation 5 minutes, temperature rise rate is 50 thereafter
oc/min, annealing time is 60 minutes, heating finishes the rear temperature vacuum annealing furnace and is made as 0
oc, furnace chamber temperature drops to lower than 55 by the time
oafter C, take out film.
2. the preparation method of a kind of magnetic recording thin film according to claim 1, is characterized in that in film, the atomic ratio of Fe atom and Pt atom is 47:53, and the volume ratio of MgO and film is 20%.
3. the preparation method of a kind of magnetic recording thin film according to claim 1 and 2, the sputtering power that it is characterized in that MgO is 95 W.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210382689.XA CN102864424B (en) | 2012-10-11 | 2012-10-11 | Preparation method of magnetic recording film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210382689.XA CN102864424B (en) | 2012-10-11 | 2012-10-11 | Preparation method of magnetic recording film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102864424A CN102864424A (en) | 2013-01-09 |
| CN102864424B true CN102864424B (en) | 2014-12-10 |
Family
ID=47443547
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210382689.XA Expired - Fee Related CN102864424B (en) | 2012-10-11 | 2012-10-11 | Preparation method of magnetic recording film |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102864424B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10741749B2 (en) | 2017-08-21 | 2020-08-11 | National University Of Singapore | Spin orbit torque-based spintronic devices using L10-ordered alloys |
| CN110120232B (en) * | 2018-02-07 | 2020-11-27 | 西南大学 | FePt-MgO magnetic recording film and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020041980A1 (en) * | 2000-10-11 | 2002-04-11 | Governor Of Akita Prefecture | Magnetic recording medium |
| CN101794600A (en) * | 2009-01-27 | 2010-08-04 | 希捷科技有限公司 | Be used to make the method for data storage medium |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100392727C (en) * | 2002-04-04 | 2008-06-04 | 富士通株式会社 | Polycrystalline structure and its production method |
| CN100510190C (en) * | 2006-11-30 | 2009-07-08 | 复旦大学 | Method for preparing c-shaft vertically aligned L10 phase FePt magnetic recording film |
| US8268462B2 (en) * | 2008-12-22 | 2012-09-18 | Seagate Technology Llc | Hybrid grain boundary additives |
-
2012
- 2012-10-11 CN CN201210382689.XA patent/CN102864424B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020041980A1 (en) * | 2000-10-11 | 2002-04-11 | Governor Of Akita Prefecture | Magnetic recording medium |
| CN101794600A (en) * | 2009-01-27 | 2010-08-04 | 希捷科技有限公司 | Be used to make the method for data storage medium |
Non-Patent Citations (2)
| Title |
|---|
| Film thickness dependence of microstructures and magnetic properties in single-layered FePt films by in-situ annealing;S.C. Chen等;《Thin Solid Films》;20110801;第519卷(第20期);第2节实验部分 * |
| S.C. Chen等.Film thickness dependence of microstructures and magnetic properties in single-layered FePt films by in-situ annealing.《Thin Solid Films》.2011,第519卷(第20期), * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102864424A (en) | 2013-01-09 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| KR100560091B1 (en) | Magnetic recording medium and magnetic recording apparatus | |
| CN104620316B (en) | The conductive substrate of FePt granule medium of the growth with (001) texture on the glass substrate | |
| US9899050B2 (en) | Multiple layer FePt structure | |
| TW584670B (en) | Fabrication of nanocomposite thin films for high density magnetic recording media | |
| JP2544586B2 (en) | Thin film magnetic recording medium, magnetic disk drive, barium ferrite thin film manufacturing method, and longitudinal magnetic recording method | |
| CN102864424B (en) | Preparation method of magnetic recording film | |
| CN102779533A (en) | FeRhPt composite film adjustable in phase transition temperature and preparation method of FeRhPt composite film | |
| CN103440875A (en) | FeRh/FePt bi-layer film for super high density heat assisted magnetic recording and preparation method thereof | |
| CN1958839A (en) | Method for preparing L10 ordered alloy film | |
| CN102194472B (en) | Super high-density perpendicular magnetic recording magnetic film and preparation method thereof | |
| CN1317695C (en) | Method for improving L10-Fept thin film performance with surface activating agent | |
| CN108060391B (en) | Method for accelerating phase transition of FePd thin film | |
| CN102061451B (en) | Preparation method of L10-FePt granular film | |
| Morisako et al. | Effect of substrate temperature on magnetic properties of strontium ferrite thin films | |
| CN102522094A (en) | Bilayer structure bottom material of SmCo5 perpendicular magnetization film and preparation method of bilayer structure bottom material | |
| JP2003006830A (en) | Magnetic recording medium and its production method | |
| JPH09232123A (en) | Hexagonal system ferrite magnetic powder | |
| US20010012573A1 (en) | Magnetic recording medium, process for fabricating magnetic recording medium and information regenerator | |
| CN107123433A (en) | A kind of spin-exchange-coupled composite magnetic recording media and preparation method thereof | |
| CN1822114A (en) | Method for preparing FePt/Ag high density magnetic recording medium material | |
| Hansen et al. | Garnets and ferrites for magneto-optical recording | |
| KR101124085B1 (en) | Magnetic recording media and fabrication method thereof | |
| JPH0619859B2 (en) | Magneto-optical recording medium | |
| TW202126837A (en) | Perpendicular magnetic recording medium with high perpendicular magnetic anisotropy and method for improving perpendicular magnetic anisotropy | |
| CN1015497B (en) | Magneto-optical disc memory alloy material and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20141210 Termination date: 20151011 |
|
| EXPY | Termination of patent right or utility model |