CN102097106B - Method for preparing c-axle vertical alignment patterned magnetic recording medium - Google Patents
Method for preparing c-axle vertical alignment patterned magnetic recording medium Download PDFInfo
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- CN102097106B CN102097106B CN2010105978493A CN201010597849A CN102097106B CN 102097106 B CN102097106 B CN 102097106B CN 2010105978493 A CN2010105978493 A CN 2010105978493A CN 201010597849 A CN201010597849 A CN 201010597849A CN 102097106 B CN102097106 B CN 102097106B
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Abstract
The invention provides a method for preparing a c-axle vertical alignment patterned magnetic recoding medium. The method comprises the following steps: 1, sputtering a buffer layer on a substrate; 2, sputtering an alignment-induced layer on the buffer layer; 3, assembling a magnetic nano-particle array on the alignment-induced layer by a dip-coating or spin-coating method; 4, sputtering a cover layer on the magnetic nano-particle array to form a support base; and 5, annealing the wafer to complete the preparation of the magnetic recording medium.
Description
Technical field:
The invention belongs to the Magnetographic Technology field, relate to the method that a kind of preparation has the shaft vertically aligned patterned magnetic recording medium of c.
Background technology:
Because the ultra paramagnetic effect of magnetic recording media, the conventional horizontal return to zero has reached theoretical limit.In order to realize the target of VHD magnetic storage; Among various record schemes are being explored; Wherein perpendicular magnetic recording (perpendicular magnetic recording; PMR), HAMR (Heat Assisted Magnetic Recording, HAMR) and patterned media (Bit-Patterned Media BPM) is considered to have most three directions of development potentiality.Wherein, It is ripe that PMR and HAMR technology are tending towards, and be widely used in the magnetic recording field of hard disks, yet this dual mode exists all defective separately: PMR can't avoid the zone of transition noise; And require each storage unit to form, make that storage unit can't continue to diminish by tens particles; HAMR then has higher requirement to heat-resisting, the heat conductivility of device and the fineness of hot secondary light source.And BPM, by means of the storage density theory expectation (1TB/in of its zero zone of transition noise and superelevation
2), especially get more and more people's extensive concerning.So-called BPM is to be arranged in order by a plurality of independently patterning magnetic cells to form, and each unit only is made up of a particle, can store the information bit of 1bit.In order to realize the storage system of BPM, there is certain requirement in storage medium: at first, each unit all will possess very high uniaxial anisotropy, and easy magnetizing axis (c axle) is wanted parallel or perpendicular to substrate surface; Secondly, the magnetic of unit upset field distribution is narrow, and the particle size distribution of promptly forming storage unit is enough even, and monodispersity is good; Once more, the low ratio of defects of sequential 2 D array be guarantee, the design of a servo-drive system and the reliability of raising information record sought with simplification.L10 phase FePt nano particle has very high magnetocrystalline anisotropy energy (6.6-10 * 10
7Erg/cm
3), can in the range scale of several nanometers, overcome superparamagnetism, show excellent stability.Therefore, use L1
0Phase FePt nano particle is the most suitable as the BPM material.At present, the method for synthetic sequential 2 D FePt nano-grain array has etching method, template and self-assembly method etc.Wherein, the etching method investment is big, cost is high, is not suitable for non-planar surfaces and carries out patterning; Template is difficult to realize the arrangement of large scale long-range order, and the template preparation section is loaded down with trivial details; Has only self-assembling method, simple, the with low cost and suitable large-scale industrial production of operation.And in the method for numerous self assemblies, inverse micelle method has especially won people's attention.Use inverse micelle method, can prepare the FePt nano-grain array that grain size is adjustable, size distribution even, standard is hexangular ordered.Yet, have the orientation stochastic distribution with the particle of the method preparation, big limitations its application in the BPM field.Someone once proposed high-intensity magnetic field and induced the method with shape anisotropy, in order to improve the oriented growth of FePt nano particle.Unfortunately the former is not suitable for suitability for industrialized production, and the orientation of particles poor that the latter obtains.And up to the present, also do not have a kind of simply and effectively way, can solve the shaft vertically aligned growth question of c of ordered FePt nano particle.
This patent has proposed a kind of brand-new growth technique, and the effect through orientation inducing layer [Au (002)] can solve L1
0The high problem of the shaft vertically aligned preparation difficulty of phase FePt nano particle ordered array c, for realizing VHD magnetic storage medium of future generation, promptly BPM provides a kind of new method.
Summary of the invention:
Fundamental purpose of the present invention is to provide a kind of preparation to have the method for the shaft vertically aligned graphical magnetic recording media of c; The particle requirement size dispersion degree of final preparation is little, it is shaft vertically aligned to be evenly distributed in order, to have c, to be suitable for the BPM material that the VHD magnetic storage is used.
The present invention proposes the method for the shaft vertically aligned patterned magnetic recording medium of a kind of c of preparation, and this method comprises:
Step 1: on substrate, sputter one deck cushion;
Step 2: sputter one deck orientation inducing layer on cushion;
Step 3: utilize the method for dip-coating or spin coating, self assembly one deck magnetic nanoparticle array on the orientation inducing layer;
Step 4: sputter one deck cap rock on the magnetic nanoparticle array forms substrate;
Step 5: substrate is carried out annealing in process, accomplish the preparation of magnetic recording media.
Wherein used substrate is MgO (a 001) single crystalline substrate.
Wherein the sputtering condition of sputter one deck orientation inducing layer is: the target spacing is 5-7cm, and working environment is an Ar atmosphere, and operating pressure is 0.1-1Pa, and the temperature of substrate 10 is 300-500 ℃, and the operating power of rf magnetron sputtering is 3-10W.
Wherein the material of cushion is Pt, and the crystal orientation is (002), and thickness is 1-4nm.
The material that wherein is orientated inducing layer is Au, and the crystal orientation is (002), and thickness is 5-50nm.
Wherein the material of cap rock is Au, and thickness is 3-10nm.
Wherein used annealing conditions is: anneal environment is 95%Ar+5%H
2Atmosphere, operating pressure are 1-10Pa, and annealing temperature is 600-700 ℃, and annealing time is 30-60 minute.
Can find out that from technique scheme the present invention has following beneficial effect:
1, the present invention utilizes the method for segmented copolymer PS-P4VP reverse micelle, on Au (002) film, has prepared thermometal FePt nano particle ordered array.Prepared FePt nanoparticle size dispersion degree is little, be evenly distributed, and grain size (3-10nm) and spacing (20-100nm) are adjustable on a large scale, are suitable as the high density magnetic storage medium.
2, the preparation method of the present invention's proposition; Be through between substrate and FePt nano particle, introducing the orientation inducing layer of layer of Au (002); Promoted the oriented growth of FePt nano particle, obtained the L10 phase FePt nano particle ordered array of c axle perpendicular to substrate surface.And, has good thermal stability because the FePt nanoparticulate dispersed in nonmagnetic Au matrix, the phenomenon of particle agglomeration can not take place in annealing process.
Description of drawings:
For further specifying technology contents of the present invention, the present invention will be described in more detail below in conjunction with accompanying drawing and embodiment, wherein:
Fig. 1 structural representation of the present invention.
Fig. 2 is the XRD figure according to embodiment of the invention sputter Au film on MgO (001) single crystalline substrate.
Fig. 3 is with (a) micella array of inverse micelle method preparation and (b) FePt nano-array relevant particle size distribution figure after the etching.
Fig. 4 is the XRD figure according to the FePt nano particle of embodiment of the invention preparation.
Fig. 5 is the FePt nano particle magnetic hysteresis loop figure according to embodiment of the invention preparation.
Embodiment
See also shown in Figure 1ly, the present invention provides a kind of c of preparation the method for shaft vertically aligned patterned magnetic recording medium, and this method comprises:
Step 1: on substrate 10, sputter one deck cushion 20, sputtering condition is: the target spacing is 5-7cm, and working environment is an Ar atmosphere, and operating pressure is 0.1-1Pa, and the temperature of substrate 10 is 300-500 ℃, the operating power of rf magnetron sputtering is 3-10W; This substrate 10 is MgO (a 001) single crystalline substrate, and the material of described cushion 20 is Pt, and the crystal orientation is (002), and thickness is 1-4nm;
Step 2: sputtering sedimentation one deck orientation inducing layer 30 on cushion 20; Sputtering condition is: the target spacing is 5-7cm, and working environment is an Ar atmosphere, and operating pressure is 0.1-1Pa; The temperature of substrate 10 is 300-500 ℃, and the operating power of rf magnetron sputtering is 3-10W; The material of described orientation inducing layer 30 is Au, and the crystal orientation is (002), and thickness is 5-50nm;
Step 3: amphiphilic block copolymer PS-P4VP is added in the toluene, fully stir, this multipolymer will be self-assembled into even, the monodispersed reverse micelle of size in toluene.Said amphiphilic block copolymer PS (the m)-concentration of P4VP (n) in toluene is about 0.5wt% (200＜m＜2000,100＜n＜300); The said well-beaten time was at least 24 hours.With slaine FeCl
3And H
2PtCl
6Add in the said inverse micellar solution, fully stir the back and combine, form the reverse micelle of slaine load after a couple of days with the P4VP kernel of reverse micelle; With slaine FeCl
3And H
2PtCl
6When adding inverse micellar solution, the size that the amount of the slaine that adds through control is regulated and control prepared FePt nano particle is between 3-10nm.Utilize the method for dip-coating or spin coating, self assembly one deck magnetic nanoparticle array 40 on orientation inducing layer 30, the pull rate of its dip-coating method is 2-40mm/min, the rotating speed of spin coating method is 500-4000r/min.
Step 4: sputter one deck cap rock 50 on magnetic nanoparticle array 40, form substrate, sputtering condition is: the target spacing is 5-7cm; Working environment is an Ar atmosphere; Operating pressure is 0.1-1Pa, and the temperature of substrate 10 is 300-500 ℃, and the operating power of rf magnetron sputtering is 3-10W; The material of this cap rock 50 is Au, and thickness is 3-10nm;
Step 5: substrate is carried out annealing in process, and annealing conditions is: anneal environment is 95%Ar+5%H
2Atmosphere, operating pressure are 1-10Pa, and annealing temperature is 600-700 ℃, and annealing time is 30-60 minute, accomplish the preparation of magnetic recording media.
Embodiment
According to the described method for preparing the shaft vertically aligned BPM of c of embodiment, come the method is described below in conjunction with specific embodiment:
1) with MgO (100) single crystalline substrate of cleaning-drying as in the magnetron sputtering chamber; The Pt that sputter one deck 2nm is thick (002) film, used sputtering condition is: the target spacing is 7cm, working environment is 0.4Pa under the Ar atmosphere; The temperature of sputter is 400 ℃, and the operating power of rf magnetron sputtering is 5W;
2) Au (002) film that sputter one deck 40nm is thick in the above again, used sputtering condition is: the target spacing is 7cm, and working environment is 0.4Pa under the Ar atmosphere, and the temperature of sputter is 400 ℃, and the operating power of rf magnetron sputtering is 5W;
3) amphiphilic block copolymer PS (1762)-P4VP (308) is added fully stirring in the toluene, the concentration of said amphiphilic block copolymer in toluene is about 0.5wt%, and the said well-beaten time is 24 hours; With slaine FeCl
3And H
2PtCl
6Add in the said inverse micellar solution, fully stir the back and combine, form the reverse micelle of slaine load after 5 days with the P4VP kernel of reverse micelle; The atomic ratio that wherein adds slaine is Fe: Pt=50: 50.
4) adopt czochralski method, the reverse micelle array of self assembly load FePt on Au (002) film, pull rate is 10mm/min.
5) the slaine load reverse micelle array of self assembly on Au (002) successively adopts oxygen and hydrogen plasma to carry out etching, removes the multipolymer parent, and makes slaine be reduced to simple substance, on substrate 10, obtains exposed FePt nanometer particle film.The power of microwave is 50W during said plasma etching, and the pressure of oxygen is 200Pa, and the time of etching is 30min, and the temperature of etching is 200 ℃.
6) in order to prevent the oxidation of particle, the thick Au film of sputter one deck 5nm on the FePt nano particle, used sputtering condition is: the target spacing is 7cm, and working environment is 1Pa under the Ar atmosphere, and the temperature of sputter is 400 ℃, and the operating power of rf magnetron sputtering is 50W;
7) at protection gas 95%Ar+5%H
2Under the state, the FePt sample that has covered the Au film is placed on is heated to 700 ℃ and kept 1 hour in the graphite furnace, be cooled to room temperature then rapidly.
Make the result:
As can beappreciated from fig. 2, directly go up epitaxial growth Au (002) film difficulty at MgO (001), the present invention has solved this problem well through introducing Pt (002) cushion.Shown in Fig. 3 (a) and (b), the FePt nano-grain array of self assembly on Au (002) film, accurate hexangular ordered.Grain size is 8nm, and spacing is 75nm, and has very narrow size distribution, and its standard deviation is merely 5%, explains that can be used as the BPM array uses.
Can find out that from the XRD figure of Fig. 4 the diffraction peak that characterizes vertical orientated FePt (001) and FePt (002) has very big intensity, the diffraction peak of other crystal faces almost cannot see on the contrary, explains that to have obtained good c-axis vertical orientated.By also finding out with the outer magnetic hysteresis loop of face in the face of Fig. 5; It is vertical orientated that annealed FePt nano particle afterwards shows good c-axis, and the outer magnetic hysteresis loop coercive force of its face is 3100 Oe, and remanence ratic is 0.52; And the coercive force in the face has only 1700 Oe, and remanence ratic is merely 0.23.In addition, calculate through the Scherrer formula, the diameter of FePt nano particle is 8nm, and the existence of Au cap rock is described, has avoided the reunion of particle effectively.
Above-described specific embodiment; The object of the invention, technical scheme and beneficial effect have been carried out further explain, and institute it should be understood that the above is merely specific embodiment of the present invention; Be not limited to the present invention; All within spirit of the present invention and principle, any modification of being made, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (5)
1. method for preparing the shaft vertically aligned patterned magnetic recording medium of c, this method comprises:
Step 1: on substrate, sputter one deck cushion;
Step 2: sputter one deck orientation inducing layer on cushion, sputtering condition is: the target spacing is 5-7cm, and working environment is an Ar atmosphere, and operating pressure is 0.1-1Pa, and substrate temperature is 300-500 ℃, the operating power of rf magnetron sputtering is 3-10W;
Step 3: the method for utilizing dip-coating or spin coating; Self assembly one deck magnetic nanoparticle array on the orientation inducing layer; This magnetic nanoparticle is through with in the amphiphilic block copolymer PS-P4VP adding toluene, fully stirs 24 hours, and this multipolymer will be self-assembled into even, the monodispersed reverse micelle of size in toluene; The concentration of this amphiphilic block copolymer in toluene is 0.5wt%, with slaine and H
2PtCl
6Add in the said inverse micellar solution, fully stir the back and combine, form the reverse micelle of slaine load after a couple of days with the P4VP kernel of reverse micelle;
Step 4: sputter one deck cap rock on the magnetic nanoparticle array forms substrate:
Step 5: substrate is carried out annealing in process, and anneal environment is 95%Ar+5%H
2Atmosphere, operating pressure are 1-10Pa, and annealing temperature is 600-700 ℃, and annealing time is 30-60 minute, accomplish the preparation of magnetic recording media.
2. the method for preparing the shaft vertically aligned patterned magnetic recording medium of c according to claim 1, wherein used substrate are MgO (001) single crystalline substrate.
3. the method for preparing the shaft vertically aligned patterned magnetic recording medium of c according to claim 1, wherein the material of cushion is Pt, and the crystal orientation is (002), and thickness is 1-4nm.
4. the method for preparing the shaft vertically aligned patterned magnetic recording medium of c according to claim 1, the material that wherein is orientated inducing layer is Au, and the crystal orientation is (002), and thickness is 5-50nm.
5. the method for preparing the shaft vertically aligned patterned magnetic recording medium of c according to claim 1, wherein the material of cap rock is Au, thickness is 3-10nm.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101217041A (en) * | 2008-01-11 | 2008-07-09 | 北京科技大学 | A preparation method for ultra-high density perpendicular magnetic recording medium |
| CN101609743A (en) * | 2008-06-18 | 2009-12-23 | 中国科学院半导体研究所 | The method for preparing parallel-oriented FePt magnetic nano-composite film |
| CN101787522A (en) * | 2010-04-02 | 2010-07-28 | 南京大学 | Method for preparing ordered magnetic nanoparticle composite film with super-high density |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101217041A (en) * | 2008-01-11 | 2008-07-09 | 北京科技大学 | A preparation method for ultra-high density perpendicular magnetic recording medium |
| CN101609743A (en) * | 2008-06-18 | 2009-12-23 | 中国科学院半导体研究所 | The method for preparing parallel-oriented FePt magnetic nano-composite film |
| CN101787522A (en) * | 2010-04-02 | 2010-07-28 | 南京大学 | Method for preparing ordered magnetic nanoparticle composite film with super-high density |
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