WO2004045793A1 - 合金ナノパーティクル及びその製造方法並びに合金ナノパーティクルを用いた磁気記録媒体 - Google Patents
合金ナノパーティクル及びその製造方法並びに合金ナノパーティクルを用いた磁気記録媒体 Download PDFInfo
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- WO2004045793A1 WO2004045793A1 PCT/JP2003/011074 JP0311074W WO2004045793A1 WO 2004045793 A1 WO2004045793 A1 WO 2004045793A1 JP 0311074 W JP0311074 W JP 0311074W WO 2004045793 A1 WO2004045793 A1 WO 2004045793A1
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/052—Metallic powder characterised by the size or surface area of the particles characterised by a mixture of particles of different sizes or by the particle size distribution
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/30—Making metallic powder or suspensions thereof using chemical processes with decomposition of metal compounds, e.g. by pyrolysis
- B22F9/305—Making metallic powder or suspensions thereof using chemical processes with decomposition of metal compounds, e.g. by pyrolysis of metal carbonyls
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y25/00—Nanomagnetism, e.g. magnetoimpedance, anisotropic magnetoresistance, giant magnetoresistance or tunneling magnetoresistance
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- G—PHYSICS
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- 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
- G11B5/68—Record carriers characterised by the selection of the material comprising one or more layers of magnetisable material homogeneously mixed with a bonding agent
- G11B5/70—Record carriers characterised by the selection of the material comprising one or more layers of magnetisable material homogeneously mixed with a bonding agent on a base layer
- G11B5/706—Record carriers characterised by the selection of the material comprising one or more layers of magnetisable material homogeneously mixed with a bonding agent on a base layer characterised by the composition of the magnetic material
- G11B5/70605—Record carriers characterised by the selection of the material comprising one or more layers of magnetisable material homogeneously mixed with a bonding agent on a base layer characterised by the composition of the magnetic material metals or alloys
- G11B5/70615—Record carriers characterised by the selection of the material comprising one or more layers of magnetisable material homogeneously mixed with a bonding agent on a base layer characterised by the composition of the magnetic material metals or alloys containing Fe metal or alloys
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- 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
- G11B5/68—Record carriers characterised by the selection of the material comprising one or more layers of magnetisable material homogeneously mixed with a bonding agent
- G11B5/70—Record carriers characterised by the selection of the material comprising one or more layers of magnetisable material homogeneously mixed with a bonding agent on a base layer
- G11B5/714—Record carriers characterised by the selection of the material comprising one or more layers of magnetisable material homogeneously mixed with a bonding agent on a base layer characterised by the dimension of the magnetic particles
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- 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
- G11B5/72—Protective coatings, e.g. anti-static or antifriction
- G11B5/727—Inorganic carbon protective coating, e.g. graphite, diamond like carbon or doped carbon
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- 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
- G11B5/7373—Non-magnetic single underlayer comprising chromium
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- 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
- G11B5/739—Magnetic recording media substrates
- G11B5/73911—Inorganic substrates
- G11B5/73913—Composites or coated substrates
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- 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
- G11B5/739—Magnetic recording media substrates
- G11B5/73911—Inorganic substrates
- G11B5/73921—Glass or ceramic substrates
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- 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
- G11B5/842—Coating a support with a liquid magnetic dispersion
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/0036—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties showing low dimensional magnetism, i.e. spin rearrangements due to a restriction of dimensions, e.g. showing giant magnetoresistivity
- H01F1/0045—Zero dimensional, e.g. nanoparticles, soft nanoparticles for medical/biological use
- H01F1/0063—Zero dimensional, e.g. nanoparticles, soft nanoparticles for medical/biological use in a non-magnetic matrix, e.g. granular solids
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
- H01F1/147—Alloys characterised by their composition
- H01F1/14708—Fe-Ni based alloys
- H01F1/14733—Fe-Ni based alloys in the form of particles
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
- Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
Definitions
- the present invention relates to an alloy nanoparticle and a method for producing the same, and a magnetic recording medium using the alloy nanoparticle. Background technology
- F e Pt expresses magnetism by ordering the crystal structure of f ee and changing it to a ⁇ ct structure. Annealing is required to perform this ordering. By annealing the substrate coated with FePt, FePt can obtain a large coercive force. In general, there is a correlation between the anneal temperature and the coercive force, and the coercive force that increases the anneal temperature increases (Science, vo1287ppl989). When subjected to high-temperature annealing, it has been reported that adjacent nanoparticles combine to form crystals with a large particle size (Applied Physics Letters, vo 179 No. 26 pp. 4 3 9 3). As the grain size increases due to the bonding of crystal grains, the average grain size of the crystal grains also increases, and the dispersion of the crystal grain sizes also increases, thus losing the advantages of nanoparticles. Disclosure of the invention
- an object of the present invention is to provide a method for producing alloy nanoparticles in which the particle size of alloy nanoparticles to be synthesized can be arbitrarily controlled.
- Another object of the present invention is to provide a magnetic recording medium in which alloy nanoparticles are applied to a recording layer without increasing the particle size and its dispersion.
- FePt alloy nanoparticles wherein the average diameter is in the range of 1 nm to 3 nm. It may contain an element selected from the group consisting of Ni, Co, Cu, Ag, Mn, and Pb, in addition to Fe and Pt.
- a method for producing alloy nanoparticles wherein the method is selected from the group consisting of hydrocarbons, alcohols, ethers, and esters having 2 to 20 carbon atoms in an inert gas atmosphere. Adding a metal salt, a reducing agent, a stabilizing ligand, and an organic iron complex to an organic solvent obtained to obtain a reaction solution; and heating the reaction solution to a predetermined temperature. And controlling the particle size of the alloy nanoparticles based on the amount of the stabilizing ligand.
- the stabilizing ligand is selected from the group consisting of carboxylic acids, sulfonic acids, sulfinic acids, phosphonic acids and amines.
- the organic iron complex is selected from F e (CO) 5, F e 2 (CO) 9 ⁇ Pi F e 3 (CO) group consisting of i 2.
- the metal salt is selected from the group consisting of bis-acetylacetonato platinum, bis-benzonitrile platinum dichloride, platinum (II) bromide, platinum (II) chloride and platinum (II) iodide. .
- a magnetic recording medium comprising: a substrate; and a FePt alloy nanoparticle disposed at substantially uniform intervals on the substrate and having an average diameter of 1 nm to 3 nm.
- a magnetic recording medium comprising: a particle layer; and a protective film formed on the FePt alloy nanoparticle layer.
- a magnetic recording medium comprising: a substrate; and a FePt alloy disposed at substantially uniform intervals on the substrate and having an average diameter of 2 nm to 10 nm.
- a nanoparticle magnetic layer containing nanoparticles, a carbon phase filled with voids between the FePt alloy nanoparticles, and a protective film formed on the nanoparticle magnetic layer.
- the ratio of the number of carbon atoms to the total number of metal atoms constituting the e Pt alloy nanoparticles and the total number of carbon atoms contained in the carbon phase is not less than 50 atomic% and less than 85 atomic%.
- a method for manufacturing a magnetic recording medium comprising: a step of preparing a FePt alloy nanoparticle, a carboxylic acid and an amine in a solvent selected from the group consisting of hexane, heptane and octane.
- a coating solution is obtained, the coating solution is applied on a substrate, and the coating solution is dried to obtain FePt alloy nanoparticles and the FePt alloy particles.
- a magnetic nanoparticle layer made of the organic mixture filling the voids between the alloy nanoparticles on the substrate, forming a salt between the carboxylic acid and the amine, and forming the magnetic nanoparticle layer into an anneal.
- the step of forming a salt between the carboxylic acid and the amine comprises maintaining the magnetic nanoparticle layer in N 2 gas for at least 5 days.
- the method comprises a step of subjecting the magnetic nanoparticle layer to beta treatment at a temperature equal to or higher than the boiling point of the solvent for 5 to 60 minutes.
- the method comprises a step of holding the magnetic nanoparticle layer in a vacuum for at least one hour.
- a method for producing a magnetic recording medium comprising: a FePt alloy nanoparticle, a carboxylic acid and a carboxylic acid, in a solvent selected from the group consisting of hexane, heptane and octane.
- a coating solution is obtained by dispersing an organic mixture containing amine, the coating solution is applied on a substrate, the coating solution is dried, and the FePt alloy nanoparticle and the FePt alloy nanoparticle are dried.
- a magnetic nanoparticle layer made of the organic mixture that fills the gap between the t-alloy nanoparticle on the substrate forming a force gap on the magnetic nanoparticle layer, and forming the magnetic nanoparticle layer on the magnetic nanoparticle layer.
- a carbon underlayer may be formed on the substrate.
- a magnetic recording medium comprising: a substrate; a carbon layer formed on the substrate; and an average particle diameter formed on the carbon layer of 2 nm to 10 nm.
- a magnetic nanoparticle layer having a particle interval within a range of 0.2 nm to 5 nm within the range, and a carbon protective film formed on the magnetic nanoparticle layer;
- a magnetic recording medium is provided, wherein the layer is composed of a plurality of nanoparticles having a particle size distribution of 10% or less and isolated from each other.
- the thickness of the carbon layer is in the range of Inm to 10 nm, and the thickness of the carbon protective film is in the range of 1 nm to 5 nm.
- FIG. 1A to 1G are graphs showing the relationship between the amount of the stabilizing ligand used and the particle size;
- FIG. 2 is a sectional configuration diagram of the perpendicular magnetic recording medium according to the first embodiment of the present invention.
- FIG. 3 is a cross-sectional configuration diagram of a longitudinal magnetic recording medium according to a second embodiment of the present invention.
- Figure 4 is a schematic diagram of the spin coater
- Figure 5 is a schematic configuration diagram of the closed bin coat device
- Figure 6 illustrates the spin-coat method
- Fig. 7A is a micrograph showing the surface state of the nanoparticle layer before annealing
- Fig. 7B is a micrograph showing the surface state of the nanoparticle layer that was aged 17 days after film formation
- Fig. 7C is a photomicrograph showing the surface state of the nanoparticle layer deposited 59 days after film formation
- Figure 8 shows the reflection F T-IR spectrum 17 days after film formation
- Figure 9 shows the reflection F T -IR spectrum on the 59th day after film formation
- Fig. 10A is a photomicrograph showing the surface state of the nanoparticle layer before annealing in a medium with a carbon cap;
- Figure 10B is a photomicrograph showing the surface state of the nanoparticle layer after annealing for 1 hour with an electron beam;
- Fig. 11A is a micrograph showing the surface state of the nanoparticle layer before annealing in a medium without carbon cap;
- Figure 11B is a micrograph showing the surface state of the nanoparticle layer after annealing for 1 hour with an electron beam;
- Fig. 12A is a micrograph showing the surface condition of the thin film after annealing
- Fig. 12B is a micrograph showing the surface condition of the thick film after annealing
- Figure 13 shows the dependence of the coercive force H c on the annealing temperature
- FIG. 14 is a photomicrograph showing the surface condition of the thin film annealed at 800 ° C .
- FIG. 15A is a micrograph showing the surface state of the nanoparticle layer after baking
- FIG. 15B is a micrograph showing the surface state of the nanoparticle layer after annealing
- FIG. 16 is a third embodiment of the present invention Sectional configuration diagram of a perpendicular magnetic recording medium according to the present invention.
- FIG. 17 is a cross-sectional configuration diagram of a surface magnetic recording medium according to a fourth embodiment of the present invention.
- FIG. 18 is a sectional configuration diagram of a perpendicular magnetic recording medium according to a fifth embodiment of the present invention.
- Figure 19A is a micrograph of the nanoparticle layer before annealing.
- Fig. 19B is a micrograph of the nanoparticle layer after annealing
- FIG. 20 is a photomicrograph of a medium without a carbon intermediate layer and a carbon protective film.
- the present invention is based on the knowledge that the saturation concentration of a metal in a reaction solution for chemically synthesizing nanoparticles can be adjusted, thereby controlling the size of the nanoparticles.
- the metal constituting the nanoparticles is added to the reaction solution, and when the concentration exceeds the saturation concentration, the formation of nanoparticles of the alloy starts. .
- the saturation concentration of the metal in the reaction solution is high, it is difficult to form aggregates of metal atoms that serve as nuclei of the nanoparticles, and as a result, the number thereof is reduced, and the individual nanoparticle grows greatly. I do.
- the particle size of the nanoparticle becomes smaller.
- the saturation concentration of the metal in the reaction solution can be changed by changing the amount of the stabilizing ligand (stabilizer) used in the synthesis reaction.
- the stabilizing ligand used in organic solvents such as ethers, alcohols, esters, and hydrocarbons. Therefore, the saturation concentration of the metal in the reaction solution depends not on the concentration of the stabilizing ligand in the reaction solution but on the absolute amount thereof. Therefore, the present invention is characterized in that the particle size of the nanoparticles is controlled by the absolute amount of the stabilizing ligand used.
- a method for producing alloy nanoparticles is as follows: In an inert gas atmosphere, a metal salt, a reducing agent, and a stable agent are used in an organic solvent selected from the group consisting of hydrocarbons, alcohols, ethers, and esters having 2 to 20 carbon atoms. Obtaining a reaction solution by adding the fluorinated ligand and the organic iron complex, and stirring the reaction solution while heating it to a predetermined temperature. Then, the particle size of the alloy nanoparticles is controlled by the amount of the stabilizing ligand.
- Usable stabilizing ligands include acids having 6 to 22 carbon atoms such as carboxylic acids, sulfonic acids, sulfinic acids, and phosphonic acids.
- a basic organic compound such as an amine also having 6 to 22 carbon atoms can be used.
- oleic acid which is a kind of carboxylic acid having a high ability to disperse metal fine particles in a liquid, and oleylamine having the same carbon chain as oleic acid and having similar chemical properties are preferable.
- These acids and amines may be used alone or in combination. They may be used together. In particular, a combination of oleic acid and oleamine is suitable.
- the heating temperature of the reaction solution is preferably in the range of 220 ° C. and 260 ° C.
- the organic Tetsu ⁇ body F e (CO) 5, F e 2 (CO) 9 some Rere is F e 3 (CO) 1 2 is suitable.
- As the metal salt bis-acetylacetona-platinum, bis-benzonitrile platinum dichloride, platinum (II) bromide, platinum (II) chloride, or platinum (II) iodide can be used. .
- the reaction solution was reacted at 230 ° C. for 30 minutes with stirring, allowed to cool to room temperature, added with 40 mL of ethanol, and centrifuged. Furthermore, a dispersion of FePt alloy nanoparticles was obtained by dispersing the precipitate in hexane. The average particle size of the FePt alloy nanoparticles obtained under these conditions was 4.3 nm.
- the particle size of the Fe et nanoparticle can be controlled by changing the amounts of oleic acid and oleylamine used in the above-mentioned synthesis reaction. Table 1 and FIGS. 1A to 3 show the particle size changes of the FePt alloy nanoparticulates obtained by changing only the amounts of oleic acid and oleylamine among the above reaction conditions.
- Figures 1A to 3 are graphs showing the effect of the amount of oleic acid and oleylamine used on the particle size of the generated FePt nanoparticles, as a function of the diameter of the nanoparticles and the frequency of occurrence. It is.
- Fig. 1A shows the particle size distribution when 0.64 mL of oleic acid and 0.68 mL of oleylamine are used, and the average particle size is 5.5 nm.
- Figure IB shows the particle size distribution when 0.32 mL of oleic acid and 0.34 mL of oleylamine were used, with an average particle size of 4.3 nm.
- Figure 1C shows the particle size distribution when 0.16 mL of oleic acid and 0.17 mL of oleylamine are used, and the average particle size is 3.3 nm.
- FIG. 1D shows the particle size distribution when 0.08 mL of oleic acid and 0.08 mL of oleamine are used, and the average particle size is 3.0 nm.
- FIG. 1E shows the particle size distribution when 0.04 mL of oleic acid and 0.04 mL of oleylamine are used, and the average particle size is 2.6 nm.
- FIG. 1F shows the particle size distribution when 0.02 mL of oleic acid and 0.02 mL of oleamine are used, and the average particle size is 2. l nm.
- Figure 1G shows the particle size distribution when using 0.1 mL of oleic acid and 0 mL of oleylamine, and the average particle size is 1.6 mL.
- the average particle size of the FePt nanoparticles can be controlled according to the amount of the stabilizing ligand added to the reaction solution. I will. That is, the amount of the stabilizing ligand used and the average particle size of the FePt nanoparticles are in a roughly proportional relationship. '
- Example 2 To the same reaction solution as in Example 1, 28.8 mg (0.11 mmo 1) of copper bisacetyl acetonate was further added.
- the same results as in Example 1 were obtained regarding the relationship between the amount of the used stabilizing ligand and the particle size.
- the nanoparticles synthesized at this time are Fe Pt Cu alloy nanoparticles.
- Example 23.4 mg (0.14 mmo 1) of silver acetate (I) was further added.
- the synthesis reaction was performed in the same manner as in Example 1 except for the other conditions. However, the same result as in Example 1 was obtained for the relationship between the amount of the used stabilizing ligand and the particle size.
- the nanoparticles synthesized at this time are FePtAg alloy nanoparticles.
- FIG. 2 a cross-sectional configuration diagram of a perpendicular magnetic recording medium 2A according to the first embodiment of the present invention employing a FePt alloy nanoparticle manufactured by the method of the present invention as a recording layer is shown. It is shown.
- a 1 A soft magnetic layer 6 such as FeSi or FeTaC is formed on a substrate 4 such as tempered glass or crystallized glass. On the soft magnetic layer 6, an intermediate layer 8 made of carbon, MgO or the like is formed.
- a FePt alloy nanoparticle layer 10 having an average diameter of 1 nm to 3 nm is formed by a chemical synthesis method.
- the FePt alloy nanoparticle layer 10 is magnetized in the vertical direction, and the FePt alloy nanoparticle 10a is arranged at substantially uniform intervals.
- a carbon protective film 12 is formed on the Fe Pt alloy nanoparticle layer 10, and a lubricant 14 is applied on the carbon protective film 12.
- FIG. 3 there is shown a cross-sectional configuration diagram of an in-plane magnetic recording medium 2B according to a second embodiment of the present invention in which a FePt alloy nanoparticle is used for a recording layer.
- An underlayer 16 made of NiP or the like is formed on a substrate 4 made of A1 tempered glass or crystallized glass.
- An intermediate layer 18 made of CrMo or the like is formed on the underlayer 16.
- a FePt alloy nanoparticle layer 20 magnetized in the in-plane direction is formed.
- the FePt alloy nanoparticles 20a have an average diameter of l nm to 3 nm and are arranged at substantially uniform intervals.
- a carbon protective film 12 is formed on the Fe Pt alloy nanoparticle layer 20, and a lubricant 14 is applied on the carbon protective film 12.
- the FePt alloy nanoparticle layers 10 and 20 are represented by Fe, Pt and Ni, Co, Cu, Ag, It may be formed of an alloy nanoparticle layer containing an element selected from the group consisting of Mn and Pb.
- the alloy nanoparticles have an average diameter of 2 nm to 6 nm, preferably 2 nm to 3 nm, and are arranged at substantially uniform intervals.
- the reason that the particle size of the nanoparticle increases during annealing is that when the alloy nanoparticle comes into contact with each other at a high temperature, the particles are fused to lower the specific surface area of the particle. This is because lowering the surface energy in this way is far more energetically advantageous than maintaining the independence of the nanoparticles.
- a means to prevent contact between nanoparticles is necessary.
- a method of mixing an organic compound that can withstand the annealing condition with a nanoparticulate dispersion liquid and applying the mixed liquid to a substrate can be mentioned.
- Organic compounds uniformly dissolved in the dispersion liquid can evenly fill the gaps between the nanoparticles after application, and the organic compounds in the gaps can be changed to amorphous carbon by appropriate annealing conditions, resulting in high durability. Can be granted.
- Examples of the organic compound suitable for the above purpose include a combination of a carboxylic acid and an amine as a basic organic compound.
- Carboxylic acid and amine can form a salt and can be firmly linked to each other, and as a result, have the effect of preventing contact between nanoproteins.
- carboxylic acid oleic acid, which is excellent as a dispersant for metal fine particles, is preferable.
- the basic organic compound to be combined with oleic acid oleic acid and the length of the main chain of the molecule are preferable. Oleamines having the same and similar chemical properties are preferred.
- the mixed state of the organic compound in the gaps between the nanoparticles can be uniform while the alloy nanoparticles are stably dispersed.
- Fe Pt alloy nanoparticles and carboxylic acid and amine are dissolved in an organic solvent such as hexane, heptane, and octane and applied to the substrate.
- the proportions of carboxylic acids and amines that form are small. Therefore, in order to effectively form a salt between carboxylic acid and amine, various methods were examined, and the following were found to be effective.
- the annealing temperature is between about 400 ° C and 900 ° C, preferably between 500 ° C and 800 ° C.
- the annealing time is about 30 minutes to about 2 hours.
- the following method can be used as a measure to suppress the fusion of FePt alloy nanoparticle particles.
- the thickness of the nanoparticle layer containing nanoparticles, carboxylic acid, and amine is set to 80 nm or less to make the film thickness uniform.
- the film thickness is 5 ⁇ ⁇ ! ⁇ 20 nm.
- a spin coating method or a dipping method can be used as a mixed solution coating method.
- a mixture containing FePt alloy nanoparticles, carboxylic acid, and amine is applied to a substrate to form a nanoparticle layer, and then sputtering and vapor deposition are performed on this nanoparticle layer. To form a carbon protective film.
- the nanoparticle layer containing the FePt alloy nanoparticle after annealing was examined.
- the ratio of the number of carbon atoms to the total number of metal atoms constituting the nanoparticles and the total number of carbon atoms filling the voids between the nanoparticles is 50 atomic% or more
- Fe P t It was found that the effect of suppressing the fusion of the nanoparticles was large. Since the magnetic properties require that the density of FePt nanoparticles in the nanoparticle layer be at least a certain level, the ratio of the number of carbon atoms must be in the range of 50 atomic% or more and less than 85%. Is preferred.
- Magnetic metals include Fe Pt alloy nanoparticles, carboxylic acid and A coating liquid in which an organic mixture composed of an amine was dispersed was used. Heptane or octane may be used instead of hexane as the organic solvent.
- the nanoparticle layer was deposited on the substrate using a spin coater as shown in Fig.4.
- FIG. 4 is a schematic configuration diagram when the spin coat device is opened, and a sealing force tap 28 through which a disk substrate rotating mechanism 26 for holding and rotating the disk substrate 24 is inserted, and a coating device.
- the sealing plate 34 passing through the liquid syringe 30 and the hexane syringe 32 forms a basic structure.
- a force-up vertical movement mechanism 36 which moves the sealing cup 28 up and down to make contact with the sealing plate 34 to form a sealed space.
- One of the contact portions between the sealing cup 28 and the sealing plate 34 is provided with an airtight sealing means such as an O-ring.
- An oil free pump 38 for evacuating the closed space to a vacuum is connected to the sealing cup 28 via a pipe.
- a sealing gauge 40 for measuring the degree of vacuum in the sealed space and a hexane vapor pressure sensor 42 for measuring the vapor pressure of hexane as the introduced solvent are arranged in the sealing power supply 28.
- the coating liquid syringe 30 is provided with a controller 31 for controlling the amount of the coating liquid dripped.
- the coating liquid syringe 30 is provided with a mechanism for linearly moving the coating liquid syringe 30 in the radial direction of the substrate 24 while maintaining the airtight structure.
- a mass flow controller 33 for controlling the amount of hexane introduced is provided in the hexane syringe 32, and a hot plate 44 is disposed below the hexane syringe 32. I have. The dropped hexane is vaporized by being heated by the hot plate 44, and the enclosed space is filled with a hexane atmosphere.
- FIG. 5 is a schematic configuration diagram of the spin coater in a closed state, in which the sealing cup 28 is moved upward by the cup vertical movement mechanism 36, and the sealing cup 28 is closed. By making contact with 4, a closed film forming chamber 50 can be formed.
- a donut shape with an outer diameter of 65 mm and an inner diameter of 2 Omm is added to the spin coater described above.
- the disk substrate 24 made of the silicon substrate was fixed to the disk substrate rotating mechanism 26 by vacuum suction, the disk substrate 24 was rotated at 300 rpm.
- the force cup vertical movement mechanism 26 is driven to move the sealing cup 28 upward, and as shown in FIG. 28 was brought into contact with a sealing plate 34 to form a sealed film forming chamber 50.
- Hexane is introduced into the sealed film forming chamber 50 by introducing 10 OmL of hexane from the hexane syringe 32, and the hexane is vaporized by heating the hot plate 44 to about 80 ° C. Then, the inside of the hermetically sealed film forming chamber 50 was previously set to a hexane atmosphere. Next, 200 ⁇ L of a coating solution in which an organic mixture containing FePt nanoparticles and a carboxylic acid and an amine were dispersed in hexane as a solvent was dispersed from a coating solution syringe 30. It was dropped for 5 seconds.
- the coating liquid was dripped while the disc substrate 24 was rotated at a slow rotation speed of 60 rpm, and the coating liquid syringe 30 was marked with an arrow in FIG.
- the solution was dropped while moving at a speed of 0.5 cm / sec in the indicated radial direction.
- the coating liquid 52 is dripped onto the disk substrate 24 in a spiral state.
- the coating liquid 52 was spread over the entire surface of the disk substrate 24 by rotating the disk substrate 24 at 100 rpm for 10 seconds.
- the hexane in the coating liquid 52 does not volatilize because the inside of the closed film forming chamber 50 is filled with hexane vapor.
- the disk substrate 24 was rotated at 300 rpm, and the gas introduction pipe 46 and the conductance pulp 4 were introduced into the sealed film formation chamber 50.
- N 2 gas was introduced at a flow rate of 10 sccm for 120 seconds through 8 to evaporate the hexane in the coating liquid 52.
- the plurality of gas introduction pipes 46 are substantially uniformly distributed in the plane, the N 2 gas is uniformly applied to the entire surface of the disk substrate 24, and the hexane is slowly and uniformly applied to the entire surface of the substrate.
- a nanoparticle film in which the FePt alloy nanoparticles are arranged in a uniform and uniform thickness.
- a nanoparticle film having a thickness of about 20 nm could be formed.
- FIG. 7A to 7C show the surface states after annealing according to the elapsed time.
- Fig. 7 A shows the surface state before annealing
- FIG. 7B shows the state after annealing 17 days after film formation
- FIG. 7C shows the state after annealing 59 days after film formation.
- the anneal conditions were as follows: anneal was carried out at 550 ° C. and at 1 ⁇ 10 4 Pa for 30 minutes.
- the composition of the nano-party cycle is F e 5 3 P t 4 7 .
- the FePt alloy nanoparticle layer was formed under the same conditions as in Example 4.
- a carbon protective film with a thickness of 5 nm was formed on the nanoparticle layer by sputtering. That is, set the sample Chiyanba, after exhaust the deposition chamber to 1 0- 5 P a, it introduces a A r to 0. 5 P a, 4 0 0 W in DC discharge was 5 nm in film A thick carbon protective film was formed.
- Fig. 10A is a TEM photograph before annealing, with a force gap
- Fig. 10B is a TEM photograph after annealing for 1 hour with an electron beam
- Fig. 11A is a TEM photograph of a sample without carbon cap before annealing
- Fig. 11B is a TEM photograph after annealing for 1 hour with an electron beam.
- the nanoparticle is annealed by the electron beam and is enlarged and aggregated.
- the sample with the carbon cap as shown in Fig. 10B, it can be seen that the aggregation of the nanoparticles did not occur.
- the carbon cap is formed on the nanoparticle layer, but the same effect can be obtained by forming the carbon underlayer on the substrate and forming the nanoparticle layer on the carbon underlayer. Can be expected.
- the FePt alloy nanoparticle layer was formed under the same conditions as in Example 4. This sample is used as a thin film sample. Next, 20 / i L of Fe Pt coating solution was dropped onto a 5 x 10 mm thermally oxidized film Si substrate and dried slowly to prepare a 150-nm thick film sample. Was. Two samples of the thin film thick film were simultaneously placed in a heat treatment furnace, heated to 700 ° C. in a vacuum, and held for 30 minutes for annealing. Fig. 12A shows a TEM photograph of the thin film surface, and Fig. 12B shows a TEM photograph of the thick film surface.
- the nanoparticles are aggregated and enlarged, whereas in the thin film shown in Fig. 12A, it is found that the nanoparticles are not aggregated.
- a variety of samples with different film thicknesses were prepared, and similar experiments were conducted. It was found that when the film thickness was 80 nm or less, no aggregation of nanoparticles was observed.
- the thickness of the nanoparticle layer is in the range of 5 nm to 201 m.
- the formation of the FePt alloy nanoparticle layer was performed under the same conditions as in Example 4 described above. In this example, it will be described that the aggregation of the nanoparticles is suppressed while obtaining a high coercive force.
- Thin film samples were collected at 600 ° C, 65 ° C, 700 ° C, and 75 ° C. Annealing was performed at 0 ° C, 800 ° C, 850 ° C, and 900 ° C for 30 minutes in a vacuum.
- Figure 13 shows the relationship between anneal temperature and coercive force.
- the thin film sample saturates at about 850 ° C and exhibits a coercivity of 6 kOe.
- FIG. 14 shows the surface state of the thin film annealed at 800 ° C.
- the coercive force of the sample without agglomeration is less than half that of the coagulated sample, but this is the result of the phenomenon of thermal fluctuation due to the small size of the nanoparticles.
- the change in coercive force with temperature is sharp due to the influence of thermal fluctuation due to the small particle size.
- the formation of the FePt alloy nanoparticle layer was performed under the same conditions as in Example 4 described above.
- a beta treatment was performed at 200 ° C. for 5 to 60 minutes in N 2 gas in order to promote the formation of a salt by combining oleic acid and oleylamine.
- Figure 15A shows the surface condition after beta.
- annealing was performed at 800 ° C. in a vacuum for 30 minutes.
- the surface condition after annealing is shown in Figure 15B. It can be seen that the nanoparticles are isolated without agglomeration even at 800 ° C. annealing because the salt is formed by the above beta treatment.
- FIG. 16 there is shown a configuration diagram of a perpendicular magnetic recording medium according to a third embodiment of the present invention in which the above-described FePt alloy nanoparticle layer is used for a recording layer.
- Components that are substantially the same as the recording media of the first and second embodiments are denoted by the same reference numerals.
- the orientation control layer 5 of the soft magnetic layer 6 is formed on the substrate 4, and the soft magnetic layer 6 is formed on the orientation control layer 5.
- An intermediate layer 8 is formed on the soft magnetic layer 6, and a nanoparticle magnetic layer 54 is formed on the intermediate layer 8.
- the nanoparticle magnetic layer 54 includes FePt alloy nanoparticle 54 a having an average diameter of 2 nm to 10 nm and amorphous carbon filled with a gap between the nanoparticle 54 a.
- the FePt alloy nanoparticles 54a are arranged at substantially uniform intervals.
- the nanoparticle magnetic layer 54 is magnetized in the vertical direction.
- a carbon protective film 12 is formed on the nanoparticle magnetic layer 54, and a lubricant 14 is applied on the carbon protective film 12.
- Fig. 17 shows the fourth embodiment of the present invention in which the FePt alloy nanoparticle layer was used as the recording layer.
- 1 shows a configuration diagram of a longitudinal magnetic recording medium according to an embodiment. Components that are substantially the same as those in the first to third embodiments are given the same reference numerals.
- An underlayer 16 made of NiP or the like is formed on the substrate 4, and an intermediate layer 18 is formed on the underlayer 16. On the intermediate layer 18, a nanoparticle magnetic layer 56 is formed.
- the nanoparticle magnetic layer 56 includes a FePt alloy nanoparticle 56 a having an average diameter of 2 nm to 10 nm, and amorphous carbon filled with a void between the nanoparticle 56 a. I have.
- the FePt alloy nanoparticles 56a are arranged at substantially uniform intervals.
- the nanoparticle magnetic layer 56 is magnetized in the in-plane direction.
- a carbon protective film 12 is formed on the nanoparticle magnetic layer 56, and a lubricant 14 is applied on the carbon protective film 12.
- FIG. 18 there is shown a configuration diagram of a perpendicular magnetic recording medium according to the fifth embodiment of the present invention, in which a magnetic nanoparticle layer is employed as a recording layer.
- a soft magnetic layer 6 made of FeTaC or the like is formed, and on the soft magnetic layer 6, a carbon intermediate layer 8 'is formed.
- the thickness of the soft magnetic layer 6 was 200 nm, and the thickness of the carbon intermediate layer 8 ′ was 5 nm, and both were formed by sputtering.
- the thickness of the middle layer 8 'is 1 nn! D preferably within the range of ⁇ 10 nm
- a magnetic nanoparticle layer 58 is formed on the carbon intermediate layer 8 '.
- the magnetic nanoparticle layer 58 was formed by a chemical synthesis method as in the above embodiments.
- the magnetic nanoparticle layer 58 contains a plurality of isolated nanoparticles 58 a having a particle size distribution of 10% or less.
- Each magnetic nanoparticle 58 a of the magnetic nanoparticle layer 58 has an average particle diameter of 2 nm to lOnm, and the particle interval is 0.2 ⁇ ! In the range of ⁇ 5 nm.
- the magnetic nanonote 58 a contains two or more elements selected from the group consisting of Fe, PtNi, Co, Cu, Ag, Mn, and Pb. Preferably, it is composed of FePt nanoparticles.
- the magnetic nanoparticle layer 58 further includes a stabilizing ligand selected from the group consisting of carboxylic acid, sulfonic acid, sulfinic acid, phosphonic acid, and amine, which fills the gap between the magnetic nanoparticles 58a. Stabilizer). Magnetic nanoparticles On the layer 58, a carbon protective film 12 is formed by a sputtering method. The carbon protective film 12 has a thickness of 1 nm to 5 nm, and has a thickness of 5 nm in the present embodiment.
- Figure 19A shows a TEM image of the nanoparticle layer before annealing.
- Figure 19B shows a TEM image of the nanoparticle after annealing.
- FIG. 20 shows a TEM image of the nanoparticle layer after annealing in a medium without the intermediate layer 8 ′ and the carbon protective film 12.
- FIG. 19B when the carbon intermediate layer 8 ′ and the carbon protective film 12 are present, no melting of the nanoparticles is observed even when annealing is performed, but the carbon intermediate layer shown in FIG. Without a carbon overcoat, the nanoparticles are melting and becoming larger.
- Table 2 shows the average particle size D before and after annealing, the standard deviation ⁇ of the particle size, and the particle size distribution ⁇ ZD.
- the average particle size D does not change before and after annealing. This is presumably because the movement of the nanoparticles was suppressed by the carbon intermediate layer 8 'and the carbon protective film 12, so that the melting of the nanoparticles was prevented.
- the medium without the carbon intermediate layer 8 ′ and the carbon protective layer 12 and the carbon intermediate layer 8 with a thickness of 5 nm were used.
- a medium without a protective film was prepared. Taking these media samples ⁇ Neil chamber one after evacuated to 3 X 1 0- 5 P a, raised at for 10 minutes until 8 0 0 ° C, The medium was kept at 800 ° C. for 30 minutes, cooled to room temperature, and a medium sample was taken out.
- Table 3 shows the average particle size D with and without the carbon intermediate layer, the standard deviation ⁇ of the particle size, and the particle size distribution ⁇ ZD.
- the amount of stabilizing ligand was halved to emphasize the effect, and the size of the nanoparticle became remarkable.
- the medium having a carbon intermediate layer has a smaller average particle size and suppresses the melting of nanoparticles. This is because the bonding between the hydrocarbon of the stabilizing ligand and the carbon intermediate layer is large, and since the hydrocarbon is carbonized by anneal and strongly bonded to the carbon intermediate layer 8 ′, the nanoparticle It is considered that the movement was suppressed, and as a result, the melting of the nanoparticles was suppressed.
- the particle size of the nanoparticles can be controlled, and the noise of the magnetic recording medium can be reduced.
- a high coercive force can be obtained while preventing aggregation and enlargement of the nanoparticles. As a result, it becomes possible to create an ultra-high density magnetic recording medium.
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Abstract
Description
Claims
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EP03811485A EP1561530A4 (en) | 2002-11-15 | 2003-08-29 | ALLOY NANOTEILES AND METHOD FOR THE PRODUCTION THEREOF AND ALLOY OF NITROUSES USING MAGNETIC RECORDING MEDIUM |
US11/046,968 US20090155630A1 (en) | 2002-11-15 | 2005-01-31 | Alloy nanoparticles, method of producing the same, and magnetic recording medium using alloy nanoparticles |
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JP2002332637A JP4164338B2 (ja) | 2002-11-15 | 2002-11-15 | 合金ナノパーティクルの製造方法 |
JP2002-332637 | 2002-11-15 |
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US11/046,968 Continuation US20090155630A1 (en) | 2002-11-15 | 2005-01-31 | Alloy nanoparticles, method of producing the same, and magnetic recording medium using alloy nanoparticles |
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US (1) | US20090155630A1 (ja) |
EP (1) | EP1561530A4 (ja) |
JP (1) | JP4164338B2 (ja) |
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WO (1) | WO2004045793A1 (ja) |
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WO2005118184A2 (en) * | 2004-04-22 | 2005-12-15 | Honda Motor Co., Ltd. | Metal and alloy nanoparticles and synthesis methods thereof |
JP2006045617A (ja) * | 2004-08-04 | 2006-02-16 | Dowa Mining Co Ltd | 磁性合金粒子の集合体 |
JP2006063347A (ja) * | 2004-07-27 | 2006-03-09 | Dowa Mining Co Ltd | 金属磁性粉およびその製造法 |
WO2011075127A1 (en) * | 2009-12-17 | 2011-06-23 | United Technologies Corporation | Method for treating a supported catalyst |
US9548501B2 (en) | 2009-12-17 | 2017-01-17 | The Research Foundation of State University Of New York Research Development Services, Binghamton University | Supported catalyst |
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JP2006299301A (ja) * | 2005-04-15 | 2006-11-02 | Nagoya Institute Of Technology | 遷移金属(Fe,Co,Ni)ナノ粒子の合成方法 |
KR100711967B1 (ko) * | 2005-08-08 | 2007-05-02 | 삼성전기주식회사 | 금속 나노 입자의 제조방법 및 도전성 잉크 |
CN100426383C (zh) * | 2005-09-02 | 2008-10-15 | 鸿富锦精密工业(深圳)有限公司 | 磁记录介质及其制作方法 |
DE102006025148A1 (de) * | 2006-05-30 | 2007-12-06 | Süd-Chemie AG | Verfahren zur Herstellung eines geträgerten Metallkatalysators |
US7807217B2 (en) * | 2006-07-05 | 2010-10-05 | Seagate Technology Llc | Method of producing self-assembled cubic FePt nanoparticles and apparatus using same |
JP4993276B2 (ja) * | 2006-12-28 | 2012-08-08 | Hoya株式会社 | 合金ナノ結晶、合金ナノ結晶の製造方法および合金ナノ結晶分散液 |
KR100905713B1 (ko) * | 2007-02-06 | 2009-07-01 | 삼성전자주식회사 | 나노결정을 이용한 정보저장매체 및 그 제조방법과,정보저장장치 |
US8419822B2 (en) * | 2008-08-18 | 2013-04-16 | Xerox Corporation | Methods for producing carboxylic acid stabilized silver nanoparticles |
US8298314B2 (en) | 2008-08-18 | 2012-10-30 | Xerox Corporation | Silver nanoparticles and process for producing same |
CN101703785B (zh) * | 2009-12-04 | 2012-05-30 | 上海师范大学 | 一种两亲超顺磁性磁共振造影剂及其制备方法 |
JP6241908B2 (ja) * | 2011-02-04 | 2017-12-06 | 国立大学法人山形大学 | 被覆金属微粒子とその製造方法 |
CN109439953B (zh) * | 2018-12-25 | 2020-03-24 | 湖北大学 | Fe43.4Pt52.3Cu4.3异质结构相多面体纳米颗粒及其制备方法和应用 |
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Also Published As
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US20090155630A1 (en) | 2009-06-18 |
JP2004169050A (ja) | 2004-06-17 |
CN1684785A (zh) | 2005-10-19 |
EP1561530A4 (en) | 2009-01-21 |
EP1561530A1 (en) | 2005-08-10 |
JP4164338B2 (ja) | 2008-10-15 |
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