WO2005022565A1 - ナノ粒子デバイス及びナノ粒子デバイスの製造方法 - Google Patents
ナノ粒子デバイス及びナノ粒子デバイスの製造方法 Download PDFInfo
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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
- H01F1/032—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 hard-magnetic materials
- H01F1/04—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 hard-magnetic materials metals or alloys
- H01F1/06—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 hard-magnetic materials metals or alloys in the form of particles, e.g. powder
- H01F1/068—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 hard-magnetic materials metals or alloys in the form of particles, e.g. powder having a L10 crystallographic structure, e.g. [Co,Fe][Pt,Pd] (nano)particles
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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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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
- C30B29/605—Products containing multiple oriented crystallites, e.g. columnar crystallites
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- 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
- H01F41/30—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 for applying nanostructures, e.g. by molecular beam epitaxy [MBE]
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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
- Y10T428/25—Web or sheet containing structurally defined element or component and including a second component containing structurally defined particles
Definitions
- Nanoparticle device and method for manufacturing nanoparticle device are described.
- the present invention relates to a nanoparticle device and a method for manufacturing a nanoparticle device, and more particularly to a perpendicular magnetic recording medium used for a hard disk in which high-density arrangement is essential.
- FePt is an alloy in which Fe and Pt have an element ratio of about 1: 1. By forming fct crystal, strong magnetic anisotropy can be imparted.
- the fct phase is an abbreviation of face centered tetragonal (face-centered square) phase.
- the fct phase in FePt basically has the same arrangement as the fee phase, but in the c-axis direction ( ⁇ 001> direction). In this structure, the Fe and Pt force Si layers appear alternately. This structure is called L1. This phase is safe at normal temperature and pressure.
- the fct phase is produced as soon as the fee phase appears in the usual production method, and it is often realized by depositing at a high temperature or annealing and cooling.
- the fee phase is an abbreviation for face centered cubic (face-centered cubic).
- face-centered cubic face-centered cubic
- FePt this phase in which Fe and Pt are randomly located at the atomic position of the fee is likely to appear.
- this phase has a magnetic anisotropy!
- the c-axis orientation is a state in which a plurality of crystallites are aligned in the ⁇ 001> direction, and is extremely important in the application of fct-FePt perpendicular magnetic recording media having magnetic anisotropy on the c-axis. .
- Out-of-plane orientation refers to the regularity of the crystal orientation in the direction perpendicular to the substrate. Even in non-epitaxial growth, surface energy can be minimized, chemical etching rate can be minimized, plasma irradiation damage can be minimized, and so on. It occurs during stress minimization and competition between orientations with different growth rates.
- In-plane orientation refers to the regularity of the crystal orientation in the horizontal direction with respect to the substrate. In non-epitaxial growth on a smooth substrate, the mechanism contributing to the in-plane orientation falls within the in-plane direction. It becomes non-oriented.
- Grain growth is a process in which a crystal grows while taking in a surrounding crystal or amorphous phase, and is a phenomenon that becomes remarkable at a high temperature, and is one of the biggest obstacles to realizing a fine structure of FePt. The temperature obtained by standardizing the process temperature with the melting point is a measure. If a high melting point material is used, the same temperature can be suppressed.
- the orientation with the minimum surface energy refers to non-epitaxial growth, which is one of the mechanisms by which the crystal orientation is aligned. Means that the internal energy of the crystallite does not depend on the orientation, and therefore tends to be aligned in a direction that minimizes the surface energy. It corresponds to the densest surface of the crystal structure.
- Heteroepitaxy is a mode in which two different types of crystals grow while maintaining the same crystal orientation relationship, and have been actively studied, including the application of quantum dots.
- the most active approach as a method for fabricating nanoparticle arrays on a substrate for realizing nanodevices is heteroepitaxial growth from a single crystal substrate.
- a crystal having a specific orientation relationship with the single crystal substrate is grown.
- the lattice constant between the single crystal substrate and the target layer is being developed by this method.
- Patent Document 1 discloses a method in which a nonmagnetic underlayer having a hep structure is formed on a nonmagnetic substrate, and a magnetic material that is an alloy containing at least Co and Pt is formed thereon.
- a technique for controlling the crystal grain size of a magnetic material and the mutual spacing of crystal grains by simultaneously supplying a certain non-magnetic material by a sputtering method to cause phase separation between the magnetic material and the oxide material is a low-temperature production technology that assumes the use of plastic resin. Due to the low temperature process, it is not possible to obtain CoPt or FePt alloys with fct structure using this technique, and large magnetic coercive force cannot be expected.
- Patent Document 1 Japanese Patent Application Laid-Open No. 2003-178413
- the orientation of the 'crystal structure' of the deposited layer greatly depends on the growth conditions. Therefore, it is necessary to obtain a microcrystalline film with controlled out-of-plane orientation, such as growing a thin film under conditions of wetting on a substrate to a surface with the minimum surface energy, or using plasma irradiation together with a surface with high resistance. Can be.
- the crystal size is determined by the balance between the melting point and the process temperature, and when combined with the melting point drop in the nano region, it is easy to produce microcrystals of around 10 nm.
- in-plane orientation is non-oriented.
- the present invention relates to a method of using the microcrystalline film obtained by this non-epitaxial growth, utilizing the surface of each microcrystal as a minute space, and producing nanoparticles for each minute space.
- the nanoparticle can be locally epitaxially grown on each base microcrystal. This is because the in-plane orientation between the microcrystals is different, making it difficult for the nanoparticle to grow over multiple microcrystals.Therefore, it is possible to grow the nanoparticles one-on-one on the underlying microcrystal. Is used. On the other hand, since the underlying microcrystals are oriented out of plane, the nanoparticles are also oriented out of plane.
- a method of laminating the nanoparticles there is a method of controlling the crystal orientation by using a polycrystalline seed layer as (1) a non-pitaxy technique. May be combined. Because of low cost, it is the most widely used method in practical use, but the size of crystal, number density, and spacing are controlled by trial and error, and controllability is low. (2) The epitaxy technique requires an expensive single-crystal substrate, and has low arbitrariness in material selection and low size controllability. (3) In the colloid particle coating and arranging method, it is difficult to control the crystal phase, and it is also difficult to control the crystal orientation, and the uniformity of a large area is low.
- An object is to provide a method for manufacturing a particle device.
- the present invention provides:
- a single-layer or multi-layer substrate an in-plane non-oriented and out-of-plane oriented microcrystalline film deposited on the substrate, and individual underlying microcrystals of the underlying microcrystalline film. And individually local epitaxy nanoparticles.
- a nanoparticle device In a nanoparticle device, a single-layer or multi-layer substrate, an in-plane non-oriented and out-of-plane oriented microcrystalline film deposited on the substrate, and individual submicrostructures of the underlying microcrystalline film
- the present invention is characterized by comprising a microcrystalline film composed of microcrystals individually local-epitaxially grown on a crystal, and nanoparticles individually local-epitaxially grown on each microcrystal of the microcrystalline film.
- nanoparticle device In a nanoparticle device, a single-layer or multi-layer substrate, an in-plane non-oriented and out-of-plane oriented underlying microcrystalline film deposited on the substrate, and individual underlying microcrystalline films of the underlying microcrystalline film Nano-particles individually local-epitaxially crystallized, microcrystalline films individually local-epitaxially grown on the nanoparticles, and laminated nanoparticles in which the nanoparticles and the microcrystalline film are repeatedly local-epitaxy in a direction perpendicular to the substrate. It is characterized by the following.
- a single-layer or multi-layer substrate an in-plane non-oriented and out-of-plane oriented microcrystalline film deposited on the substrate, and individual underlying microcrystalline films of the underlying microcrystalline film It is characterized by comprising elongated nanoparticles that are locally epitaxied individually in a crystal, and microcrystalline material that is locally epitaxied individually in the nanoparticles so as to surround the nanoparticles.
- a single-layer or multi-layer substrate an in-plane non-oriented and out-of-plane oriented microcrystalline film deposited on the substrate, and individual submicrostructures of the underlying microcrystalline film It is characterized in that it comprises vertically elongated nanoparticles individually local-epitaxially grown on a crystal, and a material different in composition from the nanoparticles, which fills the gaps between the nanoparticles.
- the nanoparticle device according to any one of [1] to [6], wherein the multilayer substrate The plate can also act as either a magnetic control layer or a structure control layer or both.
- the structure control layer is a layer that is not epitaxial with the underlying microcrystal.
- the base microcrystal and the layer that is not epitaxy are amorphous.
- the amorphous is a substance containing any one or a plurality of C, N, 0, Al, and Si.
- the base microcrystal and the epitaxy are different from each other, and the layer is a crystal having a large lattice mismatch.
- the layer is a crystal whose surface structure is disordered with the base microcrystal or epitaxy.
- the base microcrystalline film is a high melting point material.
- the high melting point material is a NaCl-type crystal.
- the NaCl-type crystal is made of a nitride.
- the nitride is TiN, VN, ZrN
- the NaCl-type crystal is an oxide.
- the oxide is MgO, CaO, Sr0, or BaO.
- the high melting point material is Ti, V, Zr,
- Nb, Mo, Hf, Ta, and W powers also increase.
- the nanoparticles are a magnetic recording material.
- the magnetic recording material has an L1 structure Is an alloy having
- the alloy having the L1 structure is f
- ct Transition metal Z is a precious metal alloy.
- the fct transition metal Z noble metal alloy is FePt or CoPt.
- nanoparticle device according to the above [3] or [4], wherein the nanoparticle is a metal alloy containing Ti, Fe, Co, Cr, Ag, Pt, etc., which is locally crystallized locally. It is characterized by being a material.
- the material different from the components of the nanoparticles is a metal'alloy material containing Ti, Fe, Co, Cr, Ag, Pt, or the like. It is characterized by the following.
- a base microcrystalline film having in-plane non-orientation and out-of-plane orientation is formed on a single-layer or multi-layer substrate by non-epitaxial growth.
- the lattice constant of the material of the microcrystalline film and the lattice constant of the nanoparticle material are matched, and the surface of each underlying microcrystal of the underlying microcrystalline film is used as a minute space, and epitaxy is locally grown on the underlying microcrystal. It is characterized in that nanoparticles are generated for each minute space.
- an in-plane non-oriented / out-of-plane oriented microcrystalline film is formed on a single-layer or multi-layer substrate by non-epitaxial growth.
- the lattice constant of the material of the microcrystalline film and the lattice constant of the nanoparticle material are matched, and the surface of each underlying microcrystal of the underlying microcrystalline film is used as a minute space, and epitaxy is locally grown on the underlying microcrystal.
- Nanoparticles are generated for each minute space, and the nanoparticle material Z and the nanoparticle material including the base material are alternately deposited in the vertical direction of the substrate on top of each other, and locally epitaxially grown, It is characterized by laminating nanoparticles.
- a base microcrystalline film having in-plane non-orientation and out-of-plane orientation is formed on a single-layer or multi-layer substrate by non-epitaxial growth. Fine connection Matching the lattice constant of the material of the crystalline film with the lattice constant of the nanoparticle material, using the surface of each underlying microcrystal of the underlying microcrystalline film as a minute space, locally growing epitaxy on the underlying microcrystal, A nanoparticle is generated every time, a material having a different composition from the nanoparticle including the base material and having the same lattice constant is deposited, segregated so that each of the nanoparticles is locally epitaxy, and the nanoparticle material and the base material are separated. Nano particles are grown in the direction perpendicular to the substrate by simultaneously or alternately depositing materials having different components from the nano particles containing the material and having the same lattice constant.
- a non-epitaxially grown non-epitaxially grown underlayer microcrystalline film is formed on a single-layer or multi-layer substrate.
- the lattice constant of the material of the microcrystalline film and the lattice constant of the nanoparticle material are matched, and the surface of each underlying microcrystal of the underlying microcrystalline film is used as a minute space, and epitaxy is locally grown on the underlying microcrystal.
- Nanoparticles are generated for each minute space, a material having a different component from the nanoparticles is deposited as powder, segregated between the nanoparticles, and the nanoparticle material and a material having a different component from the nanoparticles are simultaneously mixed.
- the nanoparticles are grown in a direction perpendicular to the substrate by alternately depositing them.
- the method for producing a nanoparticle device according to any one of [27] to [31]!
- the underlying microcrystalline film suppresses grain growth and is oriented out-of-plane at any one of minimum surface energy, minimum chemical etching rate, minimum plasma irradiation damage, minimum stress, and maximum growth rate.
- the method for producing a nanoparticle device according to any one of [27] to [32]! The nanoparticles are magnetic nanoparticles mainly composed of FePt.
- nanoparticles are magnetic nanoparticles containing CoPt as a main component.
- the crystal structure of the nanoparticle has an fct structure, and the crystal of the nanoparticle has a fct structure. 90% or more of the c-axis is oriented perpendicular to the underlying microcrystalline film.
- FIG. 1 is a manufacturing process diagram of a nanoparticle device according to a first embodiment of the present invention.
- FIG. 2 is a schematic diagram of the orientation of a base film.
- FIG. 3 is a view showing a single metal element among materials of a base film.
- FIG. 4 is a view showing an fct crystal structure of a FePt magnetic material.
- FIG. 5 is a view showing NaCl-type TiN and TaN of metal nitride as a base film.
- FIG. 6 is an electron micrograph showing a specific example of generation of FePt magnetic nanoparticles on a base film.
- FIG. 7 is a view showing a cross-sectional transmission electron microscope image of single-layer nanoparticles.
- FIG. 8 is a view showing magnetic properties (magnetization with respect to a magnetic field) of the single-layer nanoparticles in FIG. 7.
- FIG. 9 is a diagram showing magnetic properties (magnetization with respect to a magnetic field) of single-layer nanoparticles as a comparative example.
- FIG. 10 is a view showing a manufacturing process of a laminated nanoparticle device according to a second embodiment of the present invention.
- FIG. 11 is a diagram showing a cross-sectional transmission electron microscopic image of a stacked nanoparticle device according to a second embodiment of the present invention.
- FIG. 12 is a view showing a manufacturing process of a vertically long nanoparticle device according to a third embodiment of the present invention.
- FIG. 13 is a view showing a manufacturing process of a nanoparticle device composed of a vertically long nanoparticle car according to a fourth embodiment of the present invention.
- FIG. 14 is a schematic view showing the structure of a nanoparticle device according to a fifth embodiment of the present invention.
- FIG. 15 is a schematic view showing a structure of a nanoparticle device having a laminated structure FeP nanoparticle showing a sixth embodiment of the present invention.
- FIG. 16 is a schematic view showing the structure of a nanoparticle device having vertically elongated nanoparticles according to a seventh embodiment of the present invention.
- the process itself is a dry process, and the nanoparticles can be ultra-miniaturized to about 3 lOnm, and a microelectronic, magneto-optical device having nanoparticles such as a semiconductor quantum dot device can be used. Obtainable.
- the recording density of a FePt-based perpendicular magnetic recording medium which is considered as a next-generation recording medium, can be improved by one or two orders of magnitude compared to the recording density of a current hard disk. .
- the synthesized nanoparticles have a fee structure in the crystal structure, and in order to obtain a large magnetic anisotropic energy, it is necessary to increase the process temperature to obtain an fct structure.
- the aggregation of particles progresses, and particles around lOnm cannot be obtained.
- the processing temperature should be 200-1600 ° C, especially 300-800 ° C.
- the in-plane number density of the nanoparticles can be controlled independently by the crystal number density of the underlying microcrystalline film, and the volume of the nanoparticles can be controlled independently by the amount of FePt-based material deposited. Can be controlled to an appropriate distance. As a result, magnetic interference between nanoparticles can be suppressed, and the magnetic domain size, that is, the lbit size can be kept small.
- the application to a magnetic recording medium is an example, and by controlling the nanoparticle structure of size, spacing, and orientation with the underlying microcrystalline film, the function of structure control can be shared.
- the underlying microcrystalline film of the nanoparticle device on the substrate be made of a material that makes the surface that becomes epitaxy with the FePt (001) surface the surface with the smallest surface energy.
- a stable nitride film having a high melting point and preferably a Na C1 type crystal, whose surface energy is minimum, that is, the closest surface is four-fold symmetrical to the FePt (001) surface is more preferable.
- the lattice constant X of the underlying NaCl-type crystal must be smaller than the lattice constants a and c of FePt by c ⁇ 1.
- TiN having a relation of a ⁇ x ⁇ 1.la is more preferable.
- TiN and MgO in (1) and (2) above have a lattice mismatch of 9% or more with respect to the lattice constant a of FePt. If a microcrystalline film (intermediate layer) made of a material having a lattice constant between the underlying microcrystalline film and FePt is sandwiched and a local epitaxy is formed between the FePtZ intermediate layer and the Z underlying microcrystalline film, the controllability of FePt nanoparticles is further improved be able to. For example, Ag (0.
- a metal film having a high melting point material strength can be used as the underlying microcrystalline film of the nanoparticle device on the substrate.
- FePt (or CoPt) nanoparticles are grown on the above-mentioned underlying microcrystalline film under appropriate substrate heating conditions.
- the grown nanoparticles are appropriately annealed. That is, it refers to annealing including all of substrate heating film formation, heating after film formation, and substrate heating film formation and subsequent heating.
- FIG. 1 is a manufacturing process diagram of a nanoparticle device according to a first embodiment of the present invention.
- FIG. 1 (a-l) cross-sectional view
- FIG. 1 (a-2) plane view
- a Si substrate or a Si substrate 1 with a SiO film is prepared.
- a glass substrate is preferably used because it is inexpensive.
- a film (base film) 2 made of a high melting point material, for example, a TiN material is formed on a Si substrate 1 with a sputtering method.
- the high melting point material used at this time for example, TiN has a characteristic that it does not grow excessively even at room temperature or at a high temperature up to several nm even at a high temperature.
- the surface is oriented out of plane so that the surface energy is minimized, and the in-plane is not oriented.
- the film (base microcrystalline film) 2 formed in this manner is used as a base film.
- FIG. 2 is a schematic diagram of the orientation of the base film 2, in which the horizontal axis indicates the process temperature (the film formation temperature Z melting point), and the vertical axis indicates the thickness of the base film.
- the orientation in which the surface energy governed by the equilibrium theory shown in FIG. That is, in the orientation control of the base film 2 in the present invention, as shown in FIG. 2A, the orientation control is performed so that the surface energy is minimized so that the orientation matches the surface and becomes smooth.
- FIG. 2 (b) shows evolutionary selection growth, that is, although a kineticly fast plane is oriented, since irregularities are formed, it is not desirable as the orientation of the base film 2 of the present invention. .
- the unevenness of the entire base film 2 can be suppressed to several nm or less.
- the base film 2 in addition to the TiN shown in FIG. 1, as shown in FIG. 3, the base film 2 has a strong out-of-plane orientation that wets the SiO 2, High melting point material that can suppress
- Ti, Hf, Mo, Nb, Ta, V, W, and Zr region II in FIG. 3 can be used.
- a nanoparticle for example, an FePt magnetic nanoparticle having an fct structure in which the c-axis orientation is out of plane is selected. That is, as shown in Fig. 4, it is necessary to make a four-fold symmetric surface.
- the closest-packed plane and symmetry of the typical crystal structure include force (111) six-fold symmetry, bcc (l lO) two-fold symmetry, and hep (0001) six-fold symmetry. Not compatible with FePt magnetic nanoparticles.
- the closest-packed plane is the (100) plane, which has four symmetry, and matches the FePt magnetic nanoparticles.
- the nano-particle material 4 for example, a FePt magnetic material is sputtered at a high temperature. It is deposited by a method.
- the nanoparticles 4 can be locally epitaxially grown on each underlying microcrystalline film 2. This is because the in-plane orientation of the microcrystals is different, making it difficult for the nanoparticles to grow across multiple microcrystals. These are forces that take an equilibrium structure. On the other hand, since the underlying microcrystals are out-of-plane, the nanoparticles are also out-of-plane.
- a target material and a microcrystalline film that can be epitaxially grown are grown thereon, and the target material is grown in an out-of-plane direction. Nanoparticles with a controlled size can be produced.
- a FePt alloy was used, and NaCl-type TiN and TaN as metal nitrides were used as a base as shown in FIG.
- the lattice constant X is 0.4242 nm TiN
- the lattice mismatch of TiN—FePt: (001) // (001), () ⁇ ( ⁇ ) is + 9.2%
- TiN is c ⁇ a ⁇ x ⁇ l.1a, so that it is preferable as a base.
- BaO is also X 2 It has a relationship of Xa, and can be used as a base because epitaxy can be performed with a shift of 45 °.
- FIG. 6 is an electron micrograph showing a specific example of the generation of FePt magnetic nanoparticles formed on the underlayer.
- Fig. 7 shows a sample in which a TiN film was formed to 13 nm at 600 ° C on a Si substrate with a thermally oxidized film, and FePt was formed thereon at 700 ° C at a film conversion of 1.4 nm. It is a transmission electron microscope image of a cross section.
- Fig. 7 (a) From Fig. 7 (a), it can be seen that the force of FePt nanoparticles having a particle size of about 10 nm is formed at high density and at intervals.
- Fig. 7 (b) is an enlarged image, and Fig. 7 (c) is the result of further analyzing the crystal structure.
- Fig. 8 is a diagram showing the results of evaluating the magnetic properties of this sample using a SQUID (superconducting quantum interference measurement device).
- the solid line is the measurement result in the vertical direction of the substrate
- the broken line is the measurement result in the horizontal direction of the substrate. From these results, it was concluded that at room temperature, it had a coercive force of 6.2 kOe in the direction perpendicular to the substrate, 0.8 kOe in the in-plane direction, and strong magnetic anisotropy out of the plane.
- This high-density array of FePt nanoparticles with a magnetic property of around 10 nm is a promising medium for perpendicular magnetic recording.
- the present invention can be applied to CoPt magnetic nanoparticles as well as FePt magnetic nanoparticles.
- the essential conditions for a perpendicular magnetic recording medium for a hard disk include (l) fct phase (L1 structure), (2) c-axis orientation (out-of-plane or in-plane), (3) particle or crystallite size 3-10 nm, (4) structure with small contribution of interface (error prevention), (5) unevenness of several nm or less ( (6) Force that requires that the nanoparticle array has a large area and is uniform (recording area of about inch square).
- the present invention can satisfy these conditions.
- FIG. 10 is a manufacturing process diagram of a laminated nanoparticle device according to a second embodiment of the present invention.
- the high surface is placed on the Si substrate 11 with the SiO film.
- a film (base film) 12 made of a melting point material, for example, a TiN material is formed by a sputtering method.
- the high melting point material used at this time for example, TiN, grows up to several nm even at around room temperature, but has the characteristic that it does not grow excessively at high temperatures. At this time, out-of-plane orientation is performed so that surface energy is minimized, and in-plane orientation is non-oriented.
- the film (base microcrystalline film) 12 thus formed is used as a base film.
- a nanoparticle material 13 for example, a FePt magnetic material is deposited at a high temperature by a sputtering method.
- the nanoparticles 13 can be locally epitaxially grown on each underlying microcrystalline film 12. This is because the in-plane orientation differs between the microcrystals, making it difficult for the nanoparticles to grow across multiple microcrystals. It is the power to build. On the other hand, since the underlying microcrystals are out-of-plane, the nanoparticles are also out-of-plane.
- a base microcrystalline film 12 is formed thereon by a sputtering method [process similar to FIG. 10 (a)].
- a nanoparticle material 13 for example, The FePt magnetic material is deposited at a high temperature by a sputtering method. It repeats it sequentially.
- a non-epitaxial growth of a base microcrystalline film of a base microcrystalline film is performed on the substrate to form a nanoparticle of the form of nanoparticle, and the nanoparticle Z base microcrystal is formed on the substrate in the vertical direction of the substrate.
- the films are alternately deposited and local epitaxial growth is repeated.
- FIG. 11 shows a transmission electron of a cross section of a sample in which a TiN base microcrystalline film was formed on a Si substrate with a thermal oxidation film, FePt nanoparticles were further formed thereon, and a TiN base microcrystalline film was formed thereon. It is a micrograph. Local epitaxy of the FePt nanoparticles and the TiN underlying microcrystalline film is confirmed on the individual crystal grains of the TiN underlying microcrystalline film. The same structure as the TiN underlayer microcrystalline film has been realized on FePt, and by subsequently supplying FePt and TiN in the same manner, c-axis orientation and in-plane size It can be seen that the particles can be laminated.
- FIG. 12 is a view showing a manufacturing process of a nanoparticle device made of a vertically long FePt nanoparticle, showing a third embodiment of the present invention.
- a film (base film) 22 made of a high melting point material, for example, a TiN material is formed on the Si substrate 21 with the two films by a sputtering method.
- the high melting point material used at this time for example, TiN, grows up to several nm even at around room temperature, but has the characteristic that it does not grow excessively at high temperatures. At this time, out-of-plane orientation is performed so that surface energy is minimized, and in-plane orientation is non-oriented.
- the film (base microcrystalline film) 22 thus formed is used as a base film.
- a nanoparticle material 23 for example, a FePt magnetic material is deposited at a high temperature by a sputtering method.
- the nanoparticles 23 can be locally epitaxially grown on the individual underlying microcrystalline film 22. . This is because the in-plane orientation differs between the microcrystals, making it difficult for the nanoparticles to grow across multiple microcrystals. It is the power to build. On the other hand, since the underlying microcrystals are out-of-plane, the nanoparticles are also out-of-plane.
- a base microcrystalline film 22 is formed thereon by a sputtering method (process similar to FIG. 12 (a)).
- a sputtering method process similar to FIG. 12 (a)
- the ⁇ -type crystal of the base microcrystalline film is non-epitaxially grown on the substrate to form the ⁇ -type nanoparticle, and the nano-particles Z The films are alternately deposited and local epitaxial growth is repeated. Note that nanoparticle Z base microcrystals may be simultaneously deposited to cause spontaneous phase separation.
- FIG. 13 is a view showing a manufacturing process of a nanoparticle device made of a vertically long nanoparticle car according to a fourth embodiment of the present invention.
- the high surface is placed on the Si substrate 31 with the SiO film.
- a film (base film) 32 made of a melting point material, for example, a TiN material is formed by a sputtering method.
- a melting point material for example, TiN
- TiN grows up to several nm even near room temperature, but has the characteristic that it does not grow excessively at high temperatures.
- the surface is oriented out of plane so that the surface energy is minimized, and the in-plane is not oriented.
- the film (underlying microcrystalline film) 32 formed in this manner is used as an underlayer.
- a nanoparticle material 33 for example, a FePt magnetic material is deposited at a high temperature by a sputtering method.
- the nanoparticle material 33 can be locally epitaxially grown on each of the underlying microcrystalline films 32. This is because the in-plane orientation differs between the microcrystals, making it difficult for the nanoparticles to grow across multiple microcrystals.Therefore, the nanoparticles grow one-on-one on the underlying microcrystals and have an equilibrium structure in the microreaction field. Because it takes On the other hand, since the underlying microcrystals are oriented out of plane, the nanoparticles are also oriented out of plane.
- a dust (for example, an amorphous material or a metal-alloy material) 34 which is a material different from the components of the nanoparticles, is deposited thereon.
- a powder 34 an amorphous material containing any one or more of C, N, 0, Al, and Si, and a metal / alloy material containing Ti, Fe, Co, Cr, Pt, etc. are suitable. These materials have the advantage of selectively moving to the crystal grain boundaries of the ⁇ -type polycrystalline film.
- a nanoparticle material 33 for example, a FePt magnetic material is deposited thereon by a sputtering method at a high temperature. It repeats it sequentially. Note that the nanoparticle material 33 and the powder dust 34 may be simultaneously deposited.
- the underlying microcrystalline film is formed by non-epitaxial growth, an arbitrary substrate can be used. Further, when it is desired to form an underlying microcrystalline layer on a specific crystal layer, a thin amorphous material is deposited, and the underlying microcrystalline layer is formed thereon, thereby forming a crystal of the specific crystal layer.
- the underlying microcrystalline layer can be arbitrarily formed without being affected by the structure. Since the underlying microcrystalline layer is not oriented in the plane, the target nanoparticle on it is It is difficult to grow over the substrate, and local epitaxy grows one-on-one with respect to the underlying microcrystal.
- the number density of the target nanoparticles can be controlled by the crystallite number density of the underlying microcrystals, and the out-of-plane orientation of the target nanoparticles can be controlled by the out-of-plane orientation of the underlying microcrystals.
- the size of individual nanoparticles and their spacing can be controlled by adjusting the deposition amount of the desired nanoparticles. Furthermore, by filling the gap between the nanoparticles with the powder, the fusion of the nanoparticles can be prevented, and by continuing the deposition of the powder and the nanoparticle material, the nanoparticles can be continuously grown in the direction perpendicular to the substrate. In this way, the seemingly contradictory requirements of increasing the volume of individual nanoparticles while realizing a high areal density of the nanoparticles can be satisfied.
- the nanoparticle device having the structure of the FePt nanoparticle ZTiN base microcrystalline film Z substrate has been described.
- the configuration may be as follows.
- FIG. 14 is a schematic view showing the structure of a nanoparticle device according to a fifth embodiment of the present invention. As shown in FIG. 14, the distance between the FePt nanoparticles and the TiN underlying microcrystalline film is shown. A structure in which another film (microcrystalline film) is interposed may be used. For example, the Si substrate 41 with FePt nanoparticles 44ZFe microcrystalline film 43ZTiN base microcrystalline film 42ZSiO film can be used.
- FIG. 15 is a schematic diagram showing the structure of a nanoparticle device having a laminated structure FeP nanoparticle according to the sixth embodiment of the present invention.
- the microcrystals from may not necessarily be the same material as the first underlying microcrystalline film (TiN).
- the Si substrate 51 with the Fe microcrystal film 54ZFePt nanoparticle 53ZFe microcrystal film 54ZFePt nanoparticle 53ZTiN underlayer microcrystal film 52ZSiO film can be used.
- FIG. 16 is a schematic view showing the structure of a nanoparticle device having vertically elongated FeP nanoparticles according to a seventh embodiment of the present invention.
- microcrystals that locally epitaxy to the nanoparticles are used. Is not necessarily the same material as the first microcrystalline underlayer (TiN).
- TiN first microcrystalline underlayer
- the Si substrate 61 can be used.
- the force used as Fe microcrystals is not limited to this. Microcrystals other than Fe may be used. [0137] Further, the present invention is not limited to the above embodiments, but extends to the following points.
- a single-layer or multi-layer substrate an in-plane non-oriented and out-of-plane oriented microcrystalline film deposited on the substrate, and individual submicrostructures of the above-described underlying microcrystalline film.
- the crystals comprise individually locally epitaxy nanoparticles.
- nanoparticle device a single-layer or multi-layer substrate, an in-plane non-oriented and out-of-plane oriented sub-microcrystalline film deposited on the substrate, and individual sub-microstructures of the sub-microcrystalline film Nanoparticles that are individually locally epitaxy formed on crystals and laminated nanoparticles in which the base microcrystalline film and nanoparticles are repeatedly formed in a direction perpendicular to the substrate.
- nanoparticle device a single-layer or multi-layer substrate, an in-plane non-oriented and out-of-plane oriented microcrystalline film deposited on the substrate, and individual submicrostructures of the submicrocrystalline film. Elongated nanoparticles individually local-epitaxially grown on the crystal, and microcrystalline materials individually local-epitaxially grown on the nanoparticles so as to surround the nanoparticles.
- a single-layer or multi-layer substrate an in-plane non-oriented and out-of-plane oriented microcrystalline film deposited on the substrate, and an individual It comprises vertically elongated nanoparticles individually local-epitaxially grown in a crystal and a material different in composition from the nanoparticles, which fills the gaps between the nanoparticles.
- the multilayer substrate serves as one or both of a magnetic control layer and a structure control layer, and the structure control layer is a layer that is not epitaxial with the underlying microcrystal.
- the base microcrystal and the non-epitaxial layer are amorphous or a metal 'alloy', and the metal 'alloy is Ti, Fe, Co, Cr, Pt, or the like.
- the layer which is not epitaxial with the underlying microcrystalline film, is a crystal having a large lattice mismatch.
- the layer is a crystal whose surface structure is disordered.
- the base microcrystalline film is a high melting point material, and the high melting point material is a NaCl type crystal.
- the NaCl type crystal is a nitride, and the nitride is TiN, VN, ZrN, NbN, HfN, TaN, ThN.
- the NaCl-type crystal is an oxide, and the oxide is made of MgO, CaO, SrO, and BaO.
- the high melting point material is made of Ti, V, Zr, Nb, Mo, Hf, Ta, W.
- the nanoparticles are a magnetic recording material, and the magnetic recording material has a LI structure.
- the alloy having the L1 structure is a fct transition metal Z noble metal alloy.
- the fct transition metal Z precious metal alloy is FePt and CoPt.
- an in-plane non-oriented and out-of-plane oriented base microcrystalline film is formed on a single-layer or multi-layer substrate by non-epitaxial growth.
- the material of the base microcrystal film and the lattice constant of the nanoparticle material are matched, the surface of each base microcrystal of the base microcrystal film is used as a minute space, and the epitaxy is locally grown on the base microcrystal. It is characterized in that nanoparticles are generated for each space.
- a non-epitaxially grown in-plane non-oriented 'out-of-plane oriented microcrystalline film is formed on a single-layer or multi-layer substrate.
- the material of the microcrystalline film is matched with the lattice constant of the nanoparticle material, the surface of each of the underlying microcrystals of the underlying microcrystalline film is used as a minute space, and the underlying microcrystals are locally epitaxially grown.
- Nanoparticles are generated for each space, and the nanoparticle material Z and the nanoparticle material including the base material are alternately deposited on the substrate in a direction perpendicular to the substrate, and a material having a lattice constant is alternately deposited and locally grown by epitaxy. Laminate the nanoparticles.
- a non-epitaxially grown underlayer microcrystalline film is formed on a single-layer or multilayer substrate by non-epitaxial growth, and the material of the underlayer microcrystalline film is The lattice constant of the nanoparticle material is adjusted, the surface of each underlying microcrystal of the underlying microcrystal film is used as a microspace, and the epitaxy is locally grown on the underlying microcrystal, and nanoparticles are deposited for each microspace.
- a nanoparticle including the nanoparticle material and the underlayer material is deposited, and a material having a different component from the nanoparticles including the underlayer material and having a matching lattice constant is deposited, and segregated so that each of the nanoparticles is locally epitaxy.
- the nanoparticles grow in the direction perpendicular to the substrate.
- non-epitaxy is applied on a single-layer or multi-layer substrate.
- In-plane non-oriented and out-of-plane oriented underlying microcrystalline films are formed by the thermal growth, and the material of the underlying microcrystalline film and the lattice constant of the nanoparticle material are matched to each other.
- nanoparticles are grown in the vertical direction of the substrate by simultaneously or alternately depositing the nanoparticle material and a material having a different component from the nanoparticles.
- the underlying microcrystalline film suppresses grain growth and is oriented out-of-plane by any of minimum surface energy, minimum chemical etching rate, minimum plasma irradiation damage, minimum stress, and maximum growth rate.
- the nanoparticles are magnetic nanoparticles containing FePt or CoPt as a main component.
- epitaxy is locally performed by forming a sputter film under heating the substrate at 200 to 1600 ° C.
- the crystal structure of the nanoparticles has an fct structure, and 90% or more of the c-axis of the crystals of the nanoparticles are oriented perpendicular to the underlying microcrystalline film.
- the process itself is It is a lithography process that can be applied to microelectronic devices with nanoparticles such as semiconductor quantum dot devices, and is particularly suitable for hard disk perpendicular magnetic recording media where high-density arrangement is essential.
Abstract
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JP2006331582A (ja) * | 2005-05-27 | 2006-12-07 | Toshiba Corp | 垂直磁気記録媒体及び垂直磁気記録再生装置 |
JP2007026558A (ja) * | 2005-07-15 | 2007-02-01 | Univ Of Tokyo | 磁気記録媒体及びその製造方法 |
JP2009146558A (ja) * | 2007-12-14 | 2009-07-02 | Samsung Electronics Co Ltd | 磁気薄膜構造体、磁気記録媒体及びその製造方法 |
JP2013511397A (ja) * | 2009-11-30 | 2013-04-04 | インダストリー−ユニバーシティ コーポレーション ファウンデーション ソガン ユニバーシティ | ナノ粒子を柱形態で組織化させるための配列装置及びその配列方法 |
WO2013172260A1 (ja) * | 2012-05-14 | 2013-11-21 | 昭和電工株式会社 | 磁気記録媒体及び磁気記録再生装置 |
US8668833B2 (en) | 2008-05-21 | 2014-03-11 | Globalfoundries Singapore Pte. Ltd. | Method of forming a nanostructure |
JP2020080375A (ja) * | 2018-11-13 | 2020-05-28 | 東京エレクトロン株式会社 | 磁気抵抗素子の製造方法及び製造装置 |
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US8685549B2 (en) * | 2010-08-04 | 2014-04-01 | Ut-Battelle, Llc | Nanocomposites for ultra high density information storage, devices including the same, and methods of making the same |
JP6317896B2 (ja) * | 2013-07-26 | 2018-04-25 | 昭和電工株式会社 | 磁気記録媒体および磁気記憶装置 |
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