WO2004074170A1 - Materiau composite, corps structurel et son procede de fabrication film de structure polycristalline et procede de fabrication de particules - Google Patents

Materiau composite, corps structurel et son procede de fabrication film de structure polycristalline et procede de fabrication de particules Download PDF

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Publication number
WO2004074170A1
WO2004074170A1 PCT/JP2003/001875 JP0301875W WO2004074170A1 WO 2004074170 A1 WO2004074170 A1 WO 2004074170A1 JP 0301875 W JP0301875 W JP 0301875W WO 2004074170 A1 WO2004074170 A1 WO 2004074170A1
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WO
WIPO (PCT)
Prior art keywords
fine particles
magnetic
layer
substrate
nanoparticles
Prior art date
Application number
PCT/JP2003/001875
Other languages
English (en)
Japanese (ja)
Inventor
Nobutaka Ihara
Takuya Uzumaki
Atsushi Tanaka
Satoru Momose
Hiroyoshi Kodama
Original Assignee
Fujitsu Limited
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Fujitsu Limited filed Critical Fujitsu Limited
Priority to JP2004568485A priority Critical patent/JPWO2004074170A1/ja
Priority to PCT/JP2003/001875 priority patent/WO2004074170A1/fr
Publication of WO2004074170A1 publication Critical patent/WO2004074170A1/fr
Priority to US11/091,734 priority patent/US20050196606A1/en

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C30/00—Coating with metallic material characterised only by the composition of the metallic material, i.e. not characterised by the coating process
    • G—PHYSICS
    • G11—INFORMATION STORAGE
    • G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
    • G11B5/00—Recording by magnetisation or demagnetisation of a record carrier; Reproducing by magnetic means; Record carriers therefor
    • G11B5/62—Record carriers characterised by the selection of the material
    • G11B5/73—Base layers, i.e. all non-magnetic layers lying under a lowermost magnetic recording layer, e.g. including any non-magnetic layer in between a first magnetic recording layer and either an underlying substrate or a soft magnetic underlayer
    • G11B5/7368—Non-polymeric layer under the lowermost magnetic recording layer
    • G—PHYSICS
    • G11—INFORMATION STORAGE
    • G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
    • G11B5/00—Recording by magnetisation or demagnetisation of a record carrier; Reproducing by magnetic means; Record carriers therefor
    • G11B5/62—Record carriers characterised by the selection of the material
    • G11B5/73—Base layers, i.e. all non-magnetic layers lying under a lowermost magnetic recording layer, e.g. including any non-magnetic layer in between a first magnetic recording layer and either an underlying substrate or a soft magnetic underlayer
    • G11B5/7368—Non-polymeric layer under the lowermost magnetic recording layer
    • G11B5/7377—Physical structure of underlayer, e.g. texture
    • G—PHYSICS
    • G11—INFORMATION STORAGE
    • G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
    • G11B5/00—Recording by magnetisation or demagnetisation of a record carrier; Reproducing by magnetic means; Record carriers therefor
    • G11B5/84—Processes or apparatus specially adapted for manufacturing record carriers
    • G11B5/855—Coating only part of a support with a magnetic layer
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F10/00—Thin magnetic films, e.g. of one-domain structure
    • H01F10/08—Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/14—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates
    • H01F41/16—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates the magnetic material being applied in the form of particles, e.g. by serigraphy, to form thick magnetic films or precursors therefor

Definitions

  • the present invention relates to a composite material, a structure and a method for producing the same, a polycrystalline structure film and a method for producing fine particles
  • the present invention relates to a composite material, a structure and a method for producing the same, which can be used for a magnetic recording medium such as a hard disk (HD), a polycrystalline structure film, and a method for producing fine particles.
  • a magnetic recording medium such as a hard disk (HD), a polycrystalline structure film, and a method for producing fine particles.
  • nanoholes are widely known.
  • minute holes are formed, for example, on the surface of the alumina film on the substrate.
  • minute holes are regularly arranged at minute intervals.
  • the minute holes are filled with a magnetic material such as C0 or a Co-based alloy. Magnetic crystal grains are formed for each minute hole.
  • the recording density of magnetic information can be increased.
  • Magnetic recording media using iron platinum (FePt) nanoparticles have been proposed.
  • nanoparticles encapsulated in oleylamine oleate are prepared. These nanoparticles are stored in an organic solvent such as hexane. The nanoparticles are applied to a substrate of a magnetic recording medium together with an organic solvent. Thereafter, the nanoparticles are annealed. Nanoparticles crystallize based on this annealing treatment.
  • the process is performed, the fusion of nanoparticles is caused by the large thermal energy. As a result, the grains become enlarged.
  • a magnetic polycrystalline layer is widely used for the recording magnetic layer. If the crystal grain size is reduced in the magnetic polycrystalline layer, the recording density of magnetic information can be further increased.
  • a so-called seed layer that is, a fine crystal nucleus, is used to make such crystal grains fine. When the magnetic material is sputtered on the seed layer, fine crystal grains can grow from the crystal nuclei.
  • Sputtering is used to form the seed layer.
  • an ultrathin film of, for example, a metal material is formed based on the sputtering.
  • fine crystal nuclei can be formed in the ultrathin film.
  • the size and dispersion of crystal nuclei in such ultrathin films cannot be adequately controlled.
  • the size and distribution of crystal grains vary.
  • a method for producing nano metal particles based on the so-called polyol method is widely known.
  • This polyol method is widely used, for example, in producing cobalt particles.
  • Cobalt is reduced from salts such as cobalt acetate by the action of a reducing agent, diol.
  • diol a reducing agent
  • agglomeration of nanoparticles is easily caused.
  • nanoparticles of special metal alloys are manufactured, enlargement of the nanoparticles cannot be avoided.
  • Patent Document 1
  • the present invention has been made in view of the above circumstances, and an object of the present invention is to provide a composite material capable of relatively easily and uniformly filling a magnetic material in minute holes and a method for producing the same.
  • An object of the present invention is to provide a structure capable of forming finer crystal grains than ever, and a method for producing the same.
  • An object of the present invention is to provide a polycrystalline structure film capable of sufficiently controlling the size and dispersion of crystal nuclei.
  • An object of the present invention is to provide a method for producing fine and uniform fine particles relatively easily.
  • a composite material comprising: a base; and microparticles arranged in microholes formed in the surface of the base.
  • the microparticles can be reliably placed in the microholes. That is, the microparticles are completely contained in the microholes. Moreover, the position of the microhole can be controlled regularly. Based on these small holes, the small particles can be arranged regularly.
  • the microparticles are deposited in the microholes by being laminated on the surface of the substrate.
  • a confining coating layer may be formed. According to such a coating layer, the fine particles are completely contained in the fine holes. There are no microparticles on the surface of the substrate.
  • one of the substrate and the fine particles may be made of a magnetic material, and the other may be made of a non-magnetic material.
  • one of the substrate and the fine particles may be made of a conductor, and the other may be made of an insulator.
  • the fine particles may be composed of a metal element.
  • the fine particles may be composed of crystal grains.
  • an easy axis of magnetization may be established in a perpendicular direction perpendicular to the surface of the substrate.
  • the diameter of the minute holes may be set in a range of 4 nm to 50 nm, and the depth may be set in an aspect ratio of 2 to 10 nm.
  • a step of preparing a substrate having fine holes drilled on the surface a step of applying a liquid containing fine particles in a specific solvent to the surface of the substrate, Wiping off microparticles overflowing on the surface.
  • the fine particles can flow into the minute holes relatively easily. It can.
  • the microparticles can be uniformly filled in the microholes.
  • a spin coating method or a dipping method may be performed.
  • one of the substrate and the fine particles may be made of a magnetic material, and the other may be made of a non-magnetic material.
  • the diameter of the minute holes may be set to about 4 nm to 50 nm, and the depth may be set to an aspect ratio of 2 to 10 nm.
  • the above-described composite material may be used for a perpendicular magnetic recording medium such as a hard disk (HD), or may be used for other magnetic recording media.
  • a perpendicular magnetic recording medium such as a hard disk (HD)
  • HD hard disk
  • an aggregate of fine particles and a carbon atom existing between the fine particles are provided, and the carbon number is smaller than the total number of atoms constituting the fine particles and the total number of carbon atoms.
  • a structure is provided, wherein the number of atoms alone is set in the range of 45 to 96 atomic%. .
  • the diameter of such fine particles may be set in the range of 1 nm to 30 nm. Minute
  • the particles may be made of a magnetic material containing at least one of Fe, Co, and Ni.
  • the fine particles may include crystal grains.
  • a step of applying an organic solvent containing fine metal particles wrapped with the organic compound to the surface of the object, and subjecting the fine metal particles to an annealing treatment under a vacuum environment after drying the organic solvent The number of carbon atoms in the organic compound is 45 to 96 atomic% with respect to the total number of atoms constituting the fine metal particles and the number of carbon atoms in the organic compound. % Is provided in the range of%.
  • aggregation of the fine metal particles can be avoided by the action of the relatively large amount of the organic compound despite the execution of the annealing treatment.
  • the fine metal particles are maintained as fine crystal grains.
  • Such a manufacturing method may further include a step of subjecting the organic compound to a heat treatment under an inert gas atmosphere prior to performing the annealing treatment. According to such a production method, a flat surface can be established on the surface of the layer composed of the fine metal particles and the organic stabilizer, despite the increase in the amount of the organic stabilizer.
  • a polycrystalline structure film comprising a base layer, fine particles arranged on the surface of the base layer, and a crystal layer including crystal grains that grow based on the fine particles.
  • the crystal grains of the crystal layer grow based on the fine particles. Since the size and dispersion of the fine particles are sufficiently controlled, the size and distribution of the crystal grains in the crystal layer can be reliably controlled. '' In such a polycrystalline film, the fine particles only need to contain a metal element.
  • the diameter of the fine particles may be set in the range of 1 nm to 30 nm.
  • the fine particles may form a continuous layer that extends continuously on the surface of the base layer.
  • Such a polycrystalline structure film can be used for a magnetic recording medium.
  • a magnetic recording medium an underlying polycrystalline layer composed of crystal grains that grow based on fine particles and a magnetic polycrystalline layer composed of crystal grains that grow from individual crystal grains of the underlying polycrystalline layer are stacked. What is necessary is just to form a layer.
  • Such a polycrystalline structure film is used for a perpendicular magnetic recording medium.
  • a magnetic polycrystalline layer composed of crystal grains that grow based on fine particles only needs to be laminated and formed. What is necessary is just to form a layer further.
  • the crystal grains of the underlying polycrystalline layer grow based on fine particles. Since the size and dispersion of the fine particles are sufficiently controlled, the size and distribution of the crystal grains can be reliably controlled in the underlying polycrystalline layer. Since the magnetic polycrystalline layer is composed of crystal grains that grow from individual crystal grains of the underlying polycrystalline layer, the size and distribution of the crystal grains can be reliably controlled. With a magnetic recording medium, the recording density of magnetic information can be increased more than ever.
  • the fine particles may contain a metal element as described above.
  • the diameter of the fine particles may be set in the range of 1 nm to 30 nm.
  • a method for producing microparticles comprising: According to such a production method, since the reducing agent is hardly soluble in the organic solvent, the reducing agent and the organic solvent can be phase-separated. As a result of keeping the polarity of the solution low, aggregation of the fine particles can be sufficiently prevented. Fine and uniform fine particles can be formed relatively easily.
  • the metal compound may be selected from at least one of acetyl acetonate salt, a salt of an organic acid having 1 to 20 carbon atoms, bromide, and iodide.
  • the generated solution may contain two or more kinds of the metal compounds.
  • the organic solvent may be a nonprotonic organic solvent having 6 to 20 carbon atoms. These organic solvents may be selected from hydrocarbons, ethers and esters. A 1,2-diol having 2 to 6 carbon atoms may be used as the reducing agent.
  • the organic stabilizer may include a carboxylic acid R—C OOH.
  • the R in the carboxylic acid C 1 2 H 2 3, ( :. 1 7 11 3 3 Oyobi (2 1 11 4 1 if it is selected from or Re Izu Yoi organic stabilizer Amin R -. may include NH 2 this time, R in Amin is may be selected from any of C 1 3 H 2 5, C 1 8 H 3 5 and C 2 2 H 4 3.
  • the reaction temperature of the solution may be set in the range of 100 t: to 300.
  • FIG. 1 is a plan view schematically showing a specific example of a magnetic recording medium drive, that is, an internal structure of a hard disk drive (HDD).
  • HDD hard disk drive
  • FIG. 2 is an enlarged vertical sectional view showing in detail the structure of the magnetic disk according to the first embodiment of the present invention.
  • FIG. 3 is an enlarged partial cross-sectional view of the substrate schematically showing a step of forming a depression on the surface of the aluminum film.
  • FIG. 4 is an enlarged partial cross-sectional view of the substrate schematically showing a step of forming nanoholes on the surface of the substrate layer.
  • FIG. 5 is an enlarged partial cross-sectional view of the substrate schematically showing a step of applying a liquid containing nanoparticles to the surface of the substrate layer.
  • FIG. 6 is an enlarged partial cross-sectional view of the substrate schematically showing a step of wiping off nanoparticles remaining on the surface of the substrate layer.
  • FIG. 7 is an enlarged vertical sectional view showing in detail the structure of the magnetic disk according to the second embodiment of the present invention.
  • FIG. 8 is an enlarged vertical sectional view of a substrate schematically showing a step of performing a heat treatment on the liquid layer.
  • FIG. 9 is an enlarged vertical sectional view of the substrate schematically showing the structure after the liquid layer has been subjected to the heat treatment.
  • FIG. 10 is a cross-sectional view of an AFM (atomic force microscope) image of a magnetic disk according to a specific example.
  • AFM atomic force microscope
  • FIG. 11 is a cross-sectional view of an AFM image of a magnetic disk according to a comparative example.
  • FIG. 12 is an enlarged vertical sectional view showing in detail the structure of the magnetic disk according to the third embodiment of the present invention.
  • FIG. 13 is an enlarged vertical sectional view showing in detail the structure of a magnetic disk according to a modification of the third embodiment.
  • FIG. 14 is a side view schematically showing the internal structure of the spinco.
  • FIG. 15 is a table showing the relationship between the amount of the metal compound used and the composition ratio of the nanoparticles.
  • FIG. 1 schematically shows a specific example of a magnetic recording medium drive, that is, an internal structure of a hard disk drive (HDD) 11.
  • the HDD 11 includes, for example, a box-shaped housing main body 12 that partitions an internal space of a flat rectangular parallelepiped.
  • One or more magnetic disks 13 as a magnetic recording medium are accommodated in the accommodation space.
  • the magnetic disk 13 is mounted on a rotating shaft of a spindle motor 14.
  • the spindle motor 14 can rotate the magnetic disk 13 at a high speed such as, for example, 720 rpm or 1000 rpm.
  • the housing body 12 is connected with a lid (not shown) for sealing the accommodation space between the housing body 12 and the housing body 12.
  • a head shaft 16 extending vertically is fitted with a head actuator 16.
  • the head actuator 16 is composed of a rigid actuator arm 17 extending horizontally from the support shaft 15 and an actuator 17 attached to the tip of the actuator arm 17.
  • An elastic suspension 18 extending forward is provided.
  • the flying head slider 19 is cantilevered at the tip of the elastic suspension 18 by a so-called gimbal spring (not shown).
  • a pressing force is applied to the flying head slider 19 from the elastic suspension 18 toward the surface of the magnetic disk 13.
  • buoyancy acts on the flying head slider 19 by the action of the airflow generated on the surface of the magnetic disk 13. Due to the balance between the pressing force of the elastic suspension 18 and the buoyancy, the flying head slider 19 can keep flying with relatively high rigidity during the rotation of the magnetic disk 13.
  • a magnetic head that is, an electromagnetic transducer (not shown) is mounted on the flying head slider 19.
  • This electromagnetic transducer is, for example, a giant magnetoresistive (GMR) element or a tunnel junction magnetoresistive (TMR) element that reads information from a magnetic disk 13 by using the resistance change of a spin valve film or a tunnel junction film.
  • GMR giant magnetoresistive
  • TMR tunnel junction magnetoresistive
  • Element A read element and a write element such as a single magnetic pole head and an inductive write head that write information on the magnetic disk 13 using the magnetic field generated by the thin film coil pattern.
  • the flying head slider 19 can cross the surface of the magnetic disk 13 in the radial direction. Based on such movement, the electromagnetic transducer on the flying head slider 19 is positioned at a desired recording track on the magnetic disk 13.
  • the rotation of the head actuator 16 may be realized through the operation of the drive source 21 such as a voice coil motor (VCM).
  • VCM voice coil motor
  • FIG. 2 shows a cross-sectional structure of the magnetic disk 13 according to the first embodiment of the present invention in detail.
  • This magnetic disk 13 is configured as a so-called perpendicular magnetic recording medium.
  • the magnetic disk 13 includes a substrate 31 as a support, and a multilayer structure film 32 extending on the front and back surfaces of the substrate 31.
  • Substrate 3 1 are, for example, the S i body 3 3 of the disc-shaped, may be made by the S i body 3 amorphous extending 3 on the front and back surfaces S i 0 2 film 3 4.
  • a glass substrate, an aluminum substrate, or a ceramic substrate may be used as the substrate 31.
  • Magnetic information is recorded on the multilayer structure film 32.
  • the surface of the multilayer structure film 32 is covered with a protective film 35 such as a diamond-like carbon (DLC) film and a lubricating film 36 such as a perfluoropolyether (PFPE) film.
  • DLC diamond-like carbon
  • PFPE
  • the multilayer structure film 32 includes a backing layer 37 extending on the surface of the substrate 31.
  • the backing layer 37 may be made of a soft magnetic material such as a FeTaC film or a NiFe film.
  • a FeTaC film having a thickness of about 20 O nm, for example, may be used for the backing layer 37.
  • an easy axis is established in an in-plane direction defined in parallel with the surface of the substrate 31.
  • the intermediate layer 38 extends on the surface of the backing layer 37.
  • the intermediate layer 38 may be made of a nonmagnetic material such as an aluminum film.
  • the composite material, that is, the recording magnetic layer 39 is spread on the surface of the intermediate layer 38.
  • the recording magnetic layer 39 is formed by a substrate extending on the surface of the intermediate layer 38.
  • the body or substrate layer 41 is provided.
  • the substrate layer 4 1 may be employed such as alumina (A 1 2 ⁇ 3) and when was the non-magnetic material.
  • Micro holes, ie, nano holes 42 are formed in the surface of the substrate layer 41.
  • the nanoholes 42 are regularly arranged on the surface of the substrate layer 41.
  • the nanoholes 42 may be arranged, for example, along rows that are parallel at equal intervals in the circumferential direction of the substrate 31. In each row, the nanoholes 42 may be arranged at an interval equal to the interval between the rows.
  • the distance between the nanoholes 42 may be set to, for example, about 4 nm to 30 nm.
  • the diameter of the nanohole 42 may be set to about 4 nm to 50 nm.
  • the depth of the nanoholes 42 may be set based on an aspect ratio of 2 to 10. The aspect ratio indicates the ratio of the depth to the diameter of the nanohole 42.
  • Microparticles that is, nanoparticles 43 are arranged in the nanoholes 42.
  • the nanoparticles 43 contain a metal element.
  • the nanoparticles 43 need only include at least one of magnetic materials such as Fe, Co, and Ni.
  • the nanoparticles 43 may further include materials such as Cr, Pt, and Pd.
  • a magnetic FePt alloy may be used for the nanoparticles 43.
  • These nanoparticles 43 are composed of crystal grains.
  • an easy axis is established in a vertical direction perpendicular to the surface of the substrate layer 41.
  • the surface of the crystal grain is wrapped in a carbon atom (not shown).
  • carbon atoms individual grains can exist alone within nanoholes 42.
  • the crystal grains may fuse within the nanohole 42.
  • the surface of the fused grains is enveloped by carbon atoms.
  • the particle size of the nanoparticles 43 is always set to a smaller particle size than the diameter of the nanoholes 42 described above.
  • the particle size of the nanoparticles 43 may be set based on, for example, a ratio of about one-fifth to one-half of the diameter of the nanoholes 42.
  • the ratio of the standard deviation ⁇ of the particle size distribution to the average particle size D of the nanoparticles 43, that is, the particle size variance ⁇ ZD may be set to 10% or less.
  • the spacing between nanoparticles 43 within nanohole 42 is 0.2 ⁇ ! It may be set to about 5.0 nm.
  • the protective film 35 is formed on the surface of the substrate layer 41.
  • the nanoparticles 43 are confined in the nanoholes 42. That is, the protective film 35 functions as a coating layer.
  • the nanoparticles 43 are It is completely contained in the nanohole 42.
  • the nanoparticles 43 are arranged only in the nanoholes 42 and are not arranged on the surface of the substrate layer 41.
  • the direction of magnetization of the recording magnetic layer 39 can be specified based on the nanoparticles 43.
  • the nanoparticles 43 can be regularly arranged based on the nanoholes 42.
  • the outline can be clearly drawn for each individual magnetization region. So-called transition noise is suppressed.
  • the recording density of magnetic information can be reliably increased.
  • a method of manufacturing the magnetic disk 13 will be described in detail.
  • a disk-shaped substrate 31 is prepared.
  • a backing layer 37 and an aluminum layer are sequentially formed on the surface of the substrate 31.
  • a sputtering method or a vacuum evaporation method may be used.
  • nanoholes 42 are formed based on the aluminum layer.
  • the surface of the aluminum layer is oxidized.
  • the intermediate layer 38 and the substrate layer 41 are formed from the aluminum layer. Details of the method for forming the nanoholes 42 will be described later.
  • the substrate 31 is set in an annealing chamber. Within the chamber 3 X 1 0 _ 5 [P a] following the vacuum environment is established.
  • the temperature in the chamber may be set in the range of 200 ° C. to 900 ° C. For example, a temperature of 800 ° C. may be maintained for 30 minutes.
  • the temperature in the chamber is 800 from room temperature. It only has to rise to C in 10 minutes.
  • a predetermined magnetic field is applied to the nanoparticles 43.
  • the magnitude of the magnetic field may be set, for example, in the range of 0.1 to: L 0.0 [T].
  • the direction of the axis of easy magnetization is controlled by each of the nanoparticles 43.
  • the substrate 31 is cooled to room temperature.
  • a protective film 35 and a lubricating film 36 are formed on the surface of the substrate layer 41.
  • the protective film 35 may be formed by, for example, a sputtering method.
  • the lubricating film 36 may be applied based on, for example, a dipping method.
  • a method for forming the nanoholes 43 will be described in detail.
  • a rectangular pattern 45 is pressed on the surface of the aluminum film 44 on the substrate 31.
  • Protrusions 46 are formed at predetermined intervals on the surface of the cymbal shape 45.
  • Aluminum based on pressing of protrusions 4 and 6 Fine depressions 47 are formed on the surface of the film 45.
  • anodization is performed on the aluminum film 44.
  • the aluminum film 44 is immersed in an aqueous solution.
  • aqueous solution For example, 0.5 [M] of a shinic acid aqueous solution at 25 ° C is used as the aqueous solution.
  • the applied voltage is set to, for example, 40 [V].
  • the aluminum film 44 is oxidized from the surface based on the anodizing reaction.
  • the nanoholes 42 grow from the depressions 47 described above.
  • nanoholes 42 are formed on the surface of the substrate layer 41.
  • the substrate layer 41 is immersed in a phosphoric acid solution.
  • the inner peripheral surface of the nanohole 42 is etched based on the reaction with the phosphoric acid solution.
  • the diameter of the nanohole 42 is set to, for example, about 10 nm.
  • the depth of the nanoholes 42 is set to about 3 O nm.
  • the portion that is not anodized forms an aluminum intermediate layer 38.
  • the well-known super hydride method / polyol method may be used for the formation of the nanoparticles 43.
  • the diameter of the nanoparticles 43 is set to, for example, about 7 nm.
  • the individual nanoparticles 43 thus formed are enveloped with an organic compound, ie an organic stabilizer.
  • the organic stabilizer may be composed of, for example, carboxylic acid R—CO OHamine R—NH 2 .
  • R may be a linear or branched alkyl or alkenyl hydrocarbon.
  • the nanoparticles 43 wrapped in the organic stabilizer are added to a specific organic solvent.
  • the nanoparticles 43 redisperse in the organic solvent.
  • An organic solvent such as hexane, heptane or octane may be used for redispersion.
  • the substrate layer 41 having the aforementioned nanoholes 42 is prepared.
  • the formed nanoparticles 43 are filled in the nanoholes 42.
  • a liquid containing nanoparticles 43 wrapped in an organic stabilizer is applied to the surface of the base layer 41.
  • a spin coating method or a dipping method may be applied to the application.
  • the nanoparticles 43 overflowing from the nanoholes 42 to the surface of the substrate layer 41 are wiped off.
  • the substrate 31 is rotated.
  • a wiper 49 is pressed against the surface of the substrate layer 41.
  • the wiper 49 may be made of an elastic material such as rubber.
  • the nanoparticles 43 remaining on the surface of the substrate layer 41 based on the wiper 49 are reliably wiped off. like this As a result, the nanoparticles 43 are completely contained in the nanoholes 42.
  • the liquid containing the nanoparticles 43 in a specific solvent is applied to the surface of the substrate layer 41, so that the nanoparticles 43 are relatively easily formed. It can flow into the nanoholes 42. In addition, the nanoparticles 43 overflowing from the minute holes 42 to the surface of the substrate layer 41 are wiped off. The magnetic nanoparticles 43 can remain only in the nanoholes 42.
  • the recording magnetic layer 39 may be composed of the nonmagnetic substrate layer 41 and the magnetic nanoparticles 43 as described above.
  • the substrate layer 41 may be made of a magnetic material
  • the nanoparticles 43 may be made of a non-magnetic material.
  • one of the substrate layer 41 and the nanoparticles 43 may be made of a conductor, and the other may be made of an insulator.
  • FIG. 7 shows a detailed cross-sectional structure of the magnetic disk 13a according to the second embodiment of the present invention.
  • This magnetic disk 13a is configured as a so-called perpendicular magnetic recording medium.
  • the magnetic disk 13a includes a substrate 51 as a support, and a multilayer structure film 52 extending on the front and back surfaces of the substrate 51.
  • Substrate 5 for example, the S i body 3 of the disk-shaped, may be made by the S i amorphous S I_ ⁇ 2 film 5 4 over the front and back surfaces of the main body 3.
  • a glass substrate, an aluminum substrate, or a ceramic substrate may be used as the substrate 51.
  • Magnetic information is recorded on the multilayer structure film 52.
  • the surface of the multilayer structure film 52 is covered with a protective film 55 such as a diamond-like carbon (DLC) film and a lubricating film 56 such as a perfluoropolyether (PFPE) film.
  • DLC diamond-like carbon
  • PFPE perfluor
  • the multilayer structure J3 includes a backing layer 57 extending on the surface of the substrate 51.
  • the backing layer 57 may be made of a soft magnetic material such as a FeTaC film or a NiFe film.
  • the backing layer 57 has a thickness of, for example, about 200] 111?
  • an easy axis is established in an in-plane direction defined in parallel with the surface of the substrate 51.
  • the intermediate layer 58 spreads on the surface of the backing layer 57.
  • the intermediate layer 58 may be made of a non-magnetic material such as a carbon film.
  • a carbon film having a thickness of about 5 nm may be used for the intermediate layer 58.
  • the structure, that is, the recording magnetic layer 59 is spread on the surface of the intermediate layer 58.
  • the thickness of the recording magnetic layer 59 may be set to, for example, about 30 nm.
  • the recording magnetic layer 59 includes an aggregate of fine particles, that is, nano metal particles 61, which spread on the surface of the intermediate layer 58.
  • the nano metal particles 61 may be made of, for example, magnetic fine metal particles containing at least one of Fe, Co, and Ni.
  • nano metal particles 61 materials such as Pt and Pd may be added to the nano metal particles 61.
  • materials such as Pt and Pd may be added to the nano metal particles 61.
  • a magnetic FePt alloy may be used for the nano metal particles 61.
  • These nano metal particles 61 are composed of crystal grains. In each crystal grain, an easy axis of magnetization is established in a perpendicular direction perpendicular to the surface of the substrate 51.
  • the diameter of the nano metal particles 61 may be set, for example, in the range of 2 nm to 10 nm.
  • the distance between the nano metal particles 61 may be set in the range of 0.2 nm to 5.0 nm.
  • ⁇ The ratio of the standard deviation ⁇ of the particle size distribution to the average particle size D of the nano metal particles 61 That is, the particle size distribution ⁇ ZD may be set to 10% or less.
  • the recording magnetic layer 59 carbon atoms 62 exist between the nano metal particles 61.
  • the carbon atoms 62 link the nanometal particles 61 together.
  • the number of atoms of carbon atoms 62 alone is 45 atomic% to 96% of the total number of atoms constituting the nano metal particles 61 and the total number of carbon atoms 62. It is set in the range of atomic%.
  • a sputtering method or a vacuum evaporation method may be used.
  • an aggregate of nano metal particles 61 is formed on the surface of the intermediate layer 58. Details of the formation method will be described later.
  • a protective film 55 and a lubricating film 56 are formed on the surface of the aggregate of the nano metal particles 61.
  • a sputtering method may be used to form the protective film 55.
  • the lubricating film 56 may be applied based on, for example, a dip method.
  • a liquid containing the nanometal particles 61 in an organic solvent such as hexane is prepared.
  • the nano metal particles 61 may be made of, for example, an FePt alloy.
  • the diameter of the nano metal particles 61 is set to, for example, about 7 nm.
  • Individual nanometal particles 61 are wrapped with an organic compound or organic stabilizer. It is.
  • the organic stabilizer may be composed of, for example, a carboxylic acid R — C ⁇ Hamine R — NH 2 .
  • a linear or branched alkyl or alkenyl hydrocarbon may be used for R.
  • the number of carbon atoms in the organic stabilizer is in the range of 45 atomic% to 96 atomic% with respect to the total number of atoms constituting the fine metal particles and the number of carbon atoms in the organic compound. Is set by
  • the nano metal particles 61 and the organic stabilizer are coated on the surface of the intermediate layer 58 together with the organic solvent.
  • a spin coating method or a dipping method may be used. Thereafter, the organic solvent is dried.
  • the nano metal particles 61 and the organic stabilizer remain on the surface of the intermediate layer 58.
  • the distribution of the nanometal particles 61 is shaded. Irregularities are formed on the surface of the liquid layer 63 composed of the nanometal particles 61 and the organic stabilizer.
  • the surface of the intermediate layer 58 is subjected to a heat treatment.
  • the organic stabilizer is exposed to a high temperature such as 100 ° C. to 300 ° C. in an atmosphere of an inert gas such as nitrogen gas.
  • the heat treatment is continued for, for example, 1 minute to 60 minutes.
  • the distribution of the nano metal particles 61 is uniformly distributed on the surface of the intermediate layer 58.
  • a flat surface is established on the surface of the liquid layer 63 composed of the nano metal particles 61 and the organic stabilizer. Unevenness is eliminated.
  • an annealing treatment is applied to the nano metal particles 61 in a vacuum environment.
  • the substrate 51 is set in an annealing chamber.
  • a vacuum environment of 3 xl O- 5 [Pa] or less is established in the chamber.
  • the temperature inside the champer is 200 ° C to 900 ° C. What is necessary is just to set in the range of C. For example, a temperature of 800 ° C. may be maintained for 30 minutes.
  • the temperature in the chamber may be raised from room temperature to 800 in 10 minutes.
  • a predetermined magnetic field is applied to the nanometal particles 61.
  • the magnitude of the magnetic field may be set, for example, in the range of 0.1 to 10.0 [T].
  • the individual nano metal particles 61 crystallize based on the heating. By the action of the magnetic field, the easy axis of the nano metal particles 61 is aligned in a predetermined direction. Thereafter, the substrate 51 is cooled to room temperature. According to the above-described production method, the aggregation of the nano metal particles 61 can be avoided by the action of the relatively large amount of the organic stabilizer despite the execution of the annealing treatment.
  • the nano metal particles 61 are maintained as fine crystal grains. So-called magnetic domains are refined. Miniaturization of magnetic domains greatly contributes to improvement of recording density.
  • the flying head slider 19 can reliably continue to fly in a stable posture.
  • the present inventor observed an aggregate of nano metal particles 61 based on an image of FE-SEM (field emission scanning electron microscope).
  • the first specific example and the first comparative example were prepared.
  • a larger amount of the organic stabilizer than before was arranged around the nano metal particles 61.
  • a small amount of the organic stabilizer was disposed around the nanometal particles 61 in the same manner as in the past when applying the nanometal particles 61 and the organic stabilizer.
  • “small amount” means the maximum number of molecules attached around each individual nano metal particle 61.
  • the nano metal particles 61 were subjected to an annealing treatment as described above. As a result of the observation, it was confirmed that fine nano metal particles 61, that is, crystal grains were maintained in the first specific example. However, relatively large unevenness was observed on the surface of the aggregate of the nanometal particles 61. On the other hand, in the first comparative example, it was confirmed that although the flat surface was maintained on the surface of the aggregate of the nanometal particles 61, the crystal grains were enlarged based on the coalescence of the nanometal particles 61. . .
  • the present inventors observed the surface of the liquid layer 63 composed of the nanometal particles 61 and the organic stabilizer at the time of the application of the nanometal particles 61 and the organic stabilizer.
  • the first specific example and the first comparative example were used for observation.
  • irregularities were observed on the surface of the liquid layer 63. Therefore, it was demonstrated that these irregularities were maintained before and after the annealing treatment.
  • a flat surface was secured on the surface of the liquid layer 63 composed of the nanometal particles 61 and the organic stabilizer.
  • the present inventor has developed nano metal particles 6 1 based on AFM (atomic force microscope) images. Was observed.
  • AFM atomic force microscope
  • a second specific example and a second comparative example were prepared.
  • a larger amount of the organic stabilizer was disposed around the nanometal particles 61 than before in the application of the nanometal particles 61 and the organic stabilizer.
  • the annealing treatment was performed on the nano metal particles 61 in all the samples.
  • the above-described heat treatment was performed prior to the annealing treatment.
  • the nanometal particles 61 and the organic stabilizer were exposed to a high temperature of 200 ° C. for 5 minutes under a nitrogen atmosphere.
  • the second comparative example an annealing treatment was performed after the application of the nanometal particles 61 and the organic stabilizer. That is, in the second comparative example, the above-described heat treatment was not performed.
  • FIG. 10 in the second specific example, a flat surface was secured on the surface of the aggregate of the nano metal particles 61. A surface roughness Ra of 44 pm over a 1 m square was recorded. As is clear from FIG. 11, irregularities were formed on the surface of the aggregate of the nano metal particles 61 in the second comparative example. 1; surface roughness Ra of 0.909 pm on m squares was recorded.
  • the present inventor observed the aggregate of the nano metal particles 61 based on the FE-SEM image as described above.
  • Three types of samples were prepared for observation.
  • a larger amount of the organic stabilizer was disposed around the nanometal particles 61 than before in the application of the nanometal particles 61 and the organic stabilizer as in the first specific example described above.
  • the nano metal particles 61 were subjected to an annealing treatment as described above.
  • the heat treatment described above was performed prior to the annealing treatment in all samples. The heating time was set to 5 minutes, 30 minutes and 45 minutes for each sample.
  • FIG. 12 shows a cross-sectional structure of a magnetic disk 13b according to the third embodiment of the present invention in detail.
  • This magnetic disk 13b is configured as an in-plane magnetic recording medium.
  • the magnetic disk 13 b includes a substrate 71 as a support, and a polycrystalline structure film 72 extending on the front and back surfaces of the substrate 71.
  • the substrate 71 may be made of, for example, a glass substrate. However, the substrate 71 may be an aluminum substrate, a silicon substrate, or a ceramic substrate. May be used. Magnetic information is recorded on the polycrystalline structure film 72.
  • the surface of the polycrystalline structure film 72 is covered with a protective film 73 such as a diamond-like carbon (DLC) film and a lubricating film 74 such as a perfluoropolyether (PFPE) film.
  • DLC diamond-like carbon
  • PFPE perfluoropolyether
  • the polycrystalline structure film 72 includes fine particles, that is, nanoparticles 75 disposed on the surface of the base layer, that is, the substrate 71.
  • the nanoparticles 75 form a continuous layer that extends continuously on the surface of the substrate 71.
  • the thickness of the continuous layer of the nanoparticles 75 may be set to, for example, about 20 nm.
  • the nanoparticles 75 contain a metal element.
  • Such metal elements may include, for example, Fe and Pt.
  • an Fe Pt alloy may be used for the nanoparticles 75.
  • the diameter of the nanoparticles 75 may be set in the range of 2 nm to 10 nm.
  • the ratio of the standard deviation of the particle size distribution to the average particle size D of the nanoparticles 75, that is, the particle size distribution ⁇ / D may be set to 20% or less.
  • an adhesion layer 76 may be interposed between the substrate 71 and the nanoparticles 75.
  • a carbon film can be used for such an adhesion layer 76. According to the function of the adhesive film 76, the adhesive force between the substrate 71 and the nanoparticles 75 can be increased.
  • the underlying polycrystalline layer 77 spreads on the surface of the nanoparticles 75.
  • the underlying polycrystalline layer 77 is composed of crystal grains that grow based on the nanoparticle 75.
  • Base polycrystalline layer 77 may be made of, for example, an alloy containing ⁇ t and Pd.
  • a PtPd film having a thickness of about 5 nm is used for the underlying polycrystalline layer 77.
  • the magnetic polycrystalline layer 78 spreads on the surface of the base polycrystalline layer 77.
  • Magnetic polycrystalline layer 78 is composed of crystal grains that grow from individual crystal grains of base polycrystalline layer 77. Magnetic information is recorded on the magnetic polycrystalline layer 78.
  • the magnetic polycrystalline layer 78 may be made of, for example, an alloy containing at least one of Co, Ni, and Fe. Here, for example, a CoCrPt film having a thickness of about 15 nm is used.
  • the crystal grains of the underlying polycrystalline layer 77 grow based on the nanoparticles 75. Since the size and dispersion of the nanoparticles 75 are sufficiently controlled, the size and distribution of crystal grains in the underlying polycrystalline layer 77 can be reliably controlled.
  • the magnetic polycrystalline layer 7 8 is composed of crystal grains that grow from the individual crystal grains of the underlying polycrystalline layer 7 7. Therefore, the size and distribution of the crystal grains can be reliably controlled. In the magnetic disk 13b, the recording density of magnetic information can be increased more than ever.
  • a method of manufacturing the magnetic disk 13b will be briefly described.
  • a disk-shaped substrate 71 is prepared.
  • An adhesion layer 76 of carbon is formed on the surface of the substrate 71.
  • a vacuum evaporation method is used.
  • the thickness of the adhesion layer 76 may be set to, for example, about 4 nm.
  • Nanoparticles 75 are applied to the surface of the adhesion layer 76 based on a so-called spin coating method.
  • the substrate 71 is driven at a rotation speed of 300 rpm. Thereafter, the substrate 71 is placed in, for example, a hexane atmosphere. Subsequently, the rotation speed of the substrate 71 is reduced to 60 rpm. At this time, a liquid containing nanoparticles is dropped on the surface of the substrate 71 in an organic solvent. After the dropping, the rotation speed of the substrate 71 is increased to 1000 rpm. As a result of the rotation of 100 rpm being maintained for 10 seconds, the dropped liquid uniformly spreads over the surface of the substrate 71 without being tight.
  • the surface of the substrate 71 is exposed to a nitrogen gas atmosphere.
  • the hexane remaining on the surface of the substrate 71 is dried by the action of nitrogen gas.
  • a continuous film of the nanoparticles 75 is formed.
  • the nanoparticles 75 are arranged in a regular array based on so-called self-organization.
  • the substrate 71 is mounted on a sputtering device. Sputtering is performed based on the PdPt target. As a result, a PdPt alloy film, that is, an underlying polycrystalline layer 77 is formed. In the base polycrystalline layer 77, individual crystal grains grow based on the nanoparticles 75.
  • the thickness of underlying polycrystalline layer 77 may be set to, for example, about 5 nm.
  • Magnetic polycrystalline layer 78 is formed on base polycrystalline layer 77.
  • the crystal grains of the magnetic polycrystalline layer 78 grow from the crystal grains of the underlying polycrystalline layer 77 based on the epitaxial growth.
  • the thickness of the magnetic polycrystalline layer 78 may be set to, for example, about 15 nm.
  • a flask is prepared. In the flask are placed 197 mg (equivalent to 0.5 mM) of bis-acetylacetonato platinum and 39 Omg of 1,2-hexadecanediol. The flask is charged with 20 mL (milliliter) of octyl ether. Then, 0.32 mL (equivalent to 1. OmM) of oleic acid and 0.34 mL (equivalent to 1.0 mM) of oleylamine are added to the flask. Subsequently, 0.13 mL (equivalent to 1.
  • OmM of iron carbonyl Fe (CO) 5 is added to the flask.
  • the solution thus formed in the flask is stirred at a temperature of 230 ° C.
  • a diversion reaction occurs in the solution.
  • Iron platinum (FePt) nanoparticles are produced.
  • the nanoparticles are encapsulated in an organic stabilizer such as oleylamine oleate.
  • FIG. 13 shows a detailed cross-sectional structure of a magnetic disk 13c according to a modification of the third embodiment of the present invention.
  • the magnetic disk 13c is configured as a so-called perpendicular magnetic recording medium.
  • the magnetic disk 13c includes a substrate 91 as a support, and a polycrystalline structure film 92 extending on the front and back surfaces of the substrate 91.
  • the polycrystalline structure film 92 includes a backing layer 95 extending on the surface of the substrate 91.
  • the backing layer 95 may be made of a soft magnetic material such as a FeTaC film or a NiFe film.
  • an FeTaC film having a film thickness of about 20 Onm may be used for the backing layer 95.
  • an easy magnetic axis is established in an in-plane direction defined parallel to the surface of the substrate 91.
  • the polycrystalline structure film 92 includes microparticles or nanoparticles 96 disposed on the surface of the base layer or backing layer 95.
  • the nanoparticles 96 form a continuous layer, ie, a non-magnetic layer, that extends continuously on the surface of the backing layer 95.
  • the thickness of the continuous layer of the nanoparticles 96 may be set to, for example, about 20 nm.
  • the diameter of the nanoparticles 96 may be set in the range of 2 nm to 10 nm.
  • the ratio of the standard deviation ⁇ of the particle size distribution to the average particle size D of the nanoparticles 96, that is, the particle size distribution ⁇ / D may be set to 20% or less.
  • the magnetic polycrystalline layer 97 spreads on the surface of the nanoparticles 96.
  • the magnetic polycrystalline layer 97 is composed of crystal grains that grow based on the nanoparticle 96. Magnetic information is recorded on the magnetic polycrystalline layer 97.
  • the magnetic polycrystalline layer 97 may be made of, for example, an alloy containing at least one of Co, Ni, and Fe. In this case, for example, C 0 CrPt Ji-dian having a thickness of about 15 nm is used. In the magnetic polycrystalline layer 97, an easy axis of magnetization is established in a perpendicular direction perpendicular to the surface of the substrate 91.
  • an orientation control layer 98 may be interposed between the substrate 91 and the backing layer 95.
  • an orientation control layer 98 for example, Cr or an alloy film containing Cr can be used. According to the function of the orientation control film 98, the orientation of the crystal grains of the magnetic polycrystalline layer 98 can be sufficiently aligned.
  • the crystal grains of the magnetic polycrystalline layer 97 are elongated based on the nanoparticles 96. Since the size and dispersion of the nanoparticles 96 are sufficiently controlled, the size and distribution of crystal grains in the magnetic polycrystalline layer 97 can be reliably controlled.
  • a method of manufacturing the magnetic disk 13c will be briefly described.
  • a disk-shaped substrate 91 is prepared.
  • the orientation control layer 98 and the backing layer 96 may be formed on the substrate 91.
  • a sputtering method is used.
  • nanoparticles 96 are applied to the surface of the backing layer 96 based on a so-called spin coating method. A continuous film of nanoparticles 96 is formed. The nanoparticles 96 are arranged in a regular array based on the so-called self-organization.
  • the substrate 91 is mounted on a sputtering apparatus. Sputtering is performed based on the CoCrPt target. As a result, a CoCrPt alloy film, that is, a magnetic polycrystalline layer 97 is formed. In the magnetic polycrystalline layer 97, individual crystal grains grow based on the nanoparticles 96.
  • the thickness of the magnetic polycrystalline layer 97 may be set to, for example, about 15 nm.
  • FIG. 14 schematically shows the configuration of the spinco.
  • This spinco 101 has a sealed chamber 102.
  • a rotation axis 103 is arranged in the chamber 102.
  • a magnetic disk 13 (13a, 13b, 1 3 c) is accepted. With the rotation of the rotating shaft 103, the magnetic disk 13 can rotate around the central axis.
  • the first and second drip nozzles 104 and 105 face the space in the chamber 103.
  • the tip of the first dripping nozzle 104 faces the surface of the magnetic disk 13 mounted on the rotating shaft 103.
  • the first dropping nozzle 104 can move in a horizontal direction along one vertical plane including the center axis of the rotation axis 103. That is, the first dropping nozzle 104 can move in the radial direction of the magnetic disk 13 mounted on the rotating shaft 103.
  • a liquid is supplied to the first dripping nozzle 104, for example, from a predetermined liquid reservoir. Based on the combination of the rotation of the rotating shaft 103 and the horizontal movement of the first dropping nozzle 104, the liquid can be dropped on the magnetic disk 13 along, for example, a spiral path.
  • the liquid containing nanoparticles in the organic solvent may be supplied to the first dropping nozzle 104 as described above.
  • a vaporizer 106 is opposed to the tip of the second drip nozzle 105.
  • the liquid dropped from the second dropping nozzle 105 is received by the vaporizer 106.
  • the inside of the channel 102 can be filled with a gas to be vaporized by the vaporizer 106.
  • the vapor pressure of the vaporized gas is detected by the vapor pressure sensor 107.
  • the amount of the liquid dropped from the second dropping nozzle 105 can be adjusted based on the detected vapor pressure.
  • a hexane atmosphere can be established in the chamber 102 by the operation of the second dropping nozzle 105.
  • a gas inlet 108 is formed in the chamber 102.
  • the gas inlet 108 is opposed to the surface of the magnetic disk 13 mounted on the rotating shaft 103. Based on the function of the gas inlet 108, nitrogen gas can be ejected toward the surface of the magnetic disk 13 as described above.
  • a drain 109 is connected to the chamber 102. Excess liquid can be drained from the drain 109 out of the chamber 102.
  • the nanoparticles 43, 61, 75, and 96 may be produced by, for example, the following production method.
  • a nonvolatile metal compound is prepared.
  • the metal compound for example, acetyl acetonato salt can be used.
  • salts of organic acids selected from carboxylic acid salts, hydrocyanic acid salts, sulfonic acid salts, and phosphonic acid salts are used. May be. In these organic acid salts, the carbon number is set in the range of 1-20.
  • bromides and iodides can be used as the metal compound.
  • the metal element contained in such a metal compound may include, for example, Fe, Co, Ni, Pt, Cr, Cu, Ag, Mn and Pb.
  • two or more metal compounds may be included.
  • a specific organic solvent is prepared.
  • aprotic organic solvents such as hydrocarbons, ethers and esters can be used.
  • the ether includes, for example, dioctyl ether.
  • 1,2-diol can be used as the reducing agent.
  • the number of carbon atoms may be set in the range of 2 to 6.
  • 1,2-diols include, for example, 1,2-butanediol.
  • Organic stabilizers are provided for nanoparticle formation.
  • Organic stabilizers include, for example, the carboxylic acid R-COOH.
  • R in such a carboxylic acid may be selected from a linear hydrocarbon group containing a double bond.
  • Such a linear hydrocarbon group may be selected from, for example, any one of C 12 H 23 , C 17 H 33 and C 21 H 41 .
  • the organic stabilizer may include, for example, amine R—NH 2 .
  • R in such an amine may be similarly selected from a linear hydrocarbon group containing a double bond.
  • Such a linear hydrocarbon group may be selected, for example, from any of C 13 H 25 , C 18 H 35 and C 22 H 43 .
  • the organic stabilizer may include one or both of the carboxylic acid R—COOH and the amine R—NH 2 .
  • the flask is prepared in an atmosphere of an inert gas such as nitrogen gas or argon gas.
  • an inert gas such as nitrogen gas or argon gas.
  • the above-mentioned metal compound, organic solvent, reducing agent and organic stabilizer are mixed to form a solution.
  • the solution thus formed in the flask is stirred at a predetermined reaction temperature.
  • the reaction temperature is set, for example, in the range of 100 ° C to 300 ° C.
  • the metal is reduced from the metal compound in the solution based on the reducing agent.
  • nanoparticles are formed.
  • the nanoparticles are encapsulated in organic stabilizers such as oleylamine phosphate. Thereafter, the solution in the flask is cooled to room temperature.
  • a solvent such as ethanol is added into the flask.
  • the precipitate of nanoparticles and organic stabilizer is removed based on centrifugation.
  • the extracted nanoparticles and organic stabilizer are put into an organic solvent such as hexane.
  • nanoparticles dispersed in the hexane solution are obtained.
  • the reducing agent 1,2-diol is hardly soluble in aprotic organic solvents such as hydrocarbons, ethers, and esters, so that the reducing agent and the organic solvent are phase-separated.
  • aprotic organic solvents such as hydrocarbons, ethers, and esters
  • the present inventors manufactured iron platinum (FePt) nanoparticles based on the above-described manufacturing method.
  • the flask was prepared under an argon gas atmosphere.
  • a metal compound ie, 197 mg (0.5 mM equivalent) of platinum (II) acetyl acetate and 177 mg (0.5 mM equivalent) of iron (III) acetyl acetate were placed.
  • To the flask was added 1 OmL of an organic solvent, octyl ether.
  • the flask was charged with 0.9 mL of the reducing agent, ie, 1,2-butanediol.
  • an organic stabilizer 0.16 mL (equivalent to 0.05 mM) of oleic acid and 0.17 mL (equivalent to 0.5 mM) of oleylamine were added to the flask.
  • the solution thus formed in the flask was stirred at a temperature of 190 ° C for 30 minutes. Thereafter, the solution in the flask was cooled to room temperature. 1 OmL of ethanol was added to the flask. The precipitate of nanoparticles and organic stabilizer was removed based on centrifugation. The extracted nanoparticles and organic stabilizer were injected into a hexane solution. Thus, FePt nanoparticles dispersed in the hexane solution were obtained.
  • the present inventors have verified the FePt nanoparticles formed as described above. As a result, it was confirmed that the average particle size of the FePt nanoparticles was about 2.9 nm. That is, it was confirmed that very fine and uniform nanoparticles were formed. It was confirmed that the composition ratio Fe: Pt of the FePt nanoparticles was 45:55 [%].
  • the present inventors examined the relationship between the amount of the metal compound used and the composition ratio of the nanoparticles.
  • platinum (II) acetate Ruacetonato and iron (III) acetilacetonato were used.
  • the inventor changed the amount of each metal compound used.
  • the composition ratio of Fe Pt nanoparticles can reflect the ratio of the amount of platinum (II) acetyl acetonato used to the amount of iron (III) acetyl acetonato used. confirmed. That is, according to the above-described production method, the composition ratio of the metal in the nanoparticles can be controlled based on the amount of the metal compound used.
  • platinum (II) acetyl acetonate is composed of platinum (II) acetate, platinum benzoate (11), platinum cyanide (11), platinum benzenesulfonate ( I 1), platinum propylphosphonate (1 1), platinum bromide (1 1), and platinum iodide (II) were confirmed to be replaced.
  • iron (III) acetyla settonate is composed of iron (III) acetate, iron benzoate (111), iron cyanide (111), iron benzenesulfonate (II1), iron propylphosphonate (II).
  • the present inventors produced nanoparticles based on platinum (II) acetyl acetonato, iron (III) acetyl acetonato and bis (acetyl acetonato copper) according to the above-mentioned production method.
  • platinum (II) acetyl acetonato, iron (III) acetyl acetonato and bis (acetyl acetonato copper) according to the above-mentioned production method.
  • white gold-iron-copper (FePtCu) nanoparticles with an average particle size of 2.7 nm to 3.5 nm were obtained. It was confirmed that the composition ratio of the platinum-iron-copper nanoparticles reflects the amount of each metal compound used.
  • the present inventors produced nanoparticles based on platinum (II) acetyl acetonato, iron (III) acetyl acetonato and silver (I) acetate according to the above-mentioned production method.
  • platinum-iron-silver (PtFeAg) nanoparticles with an average particle size of 2.6 nm to 3.4 nm were obtained. It was confirmed that the composition ratio of platinum iron silver nanoparticles reflects the amount of each metal compound used.
  • the inventor produced nanoparticles based on the above-mentioned production method.
  • the metal compounds include platinum (II) acetylacetonato and iron (III)
  • cobalt I) acetyl acetonatochrome
  • III cobalt
  • acetyl acetonatochrome III
  • acetyl acetonato nickel
  • II acetyl acetonato
  • mangan II) acetyla Either setnat or lead (II) acetyl acetonato was used.
  • FePtCo nanoparticles, FePtCr nanoparticles, FePtNi nanoparticles, FePtMn nanoparticles, and FePtPb nanoparticles with average particle sizes of 2.6 nm to 3.6 nm were obtained.
  • the composition ratio of these nanoparticles reflects the amount of each metal compound used.

Abstract

L'invention porte sur un matériau composite (39) comprenant un substrat non magnétique (41) dont la surface est percée des microtrous (42) remplis de particules magnétiques (43) y étant solidement logés. La position des microtrous peut être réglée régulièrement et les particules (43) peuvent être régulièrement disposés dans les microtrous (42).
PCT/JP2003/001875 2003-02-20 2003-02-20 Materiau composite, corps structurel et son procede de fabrication film de structure polycristalline et procede de fabrication de particules WO2004074170A1 (fr)

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PCT/JP2003/001875 WO2004074170A1 (fr) 2003-02-20 2003-02-20 Materiau composite, corps structurel et son procede de fabrication film de structure polycristalline et procede de fabrication de particules
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