Classifications

• • 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
  • H01F1/20—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 in the form of particles, e.g. powder
  • H01F1/22—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 in the form of particles, e.g. powder pressed, sintered, or bound together
  • H01F1/24—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 in the form of particles, e.g. powder pressed, sintered, or bound together the particles being insulated
  • H01F1/26—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 in the form of particles, e.g. powder pressed, sintered, or bound together the particles being insulated by macromolecular organic substances
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B22—CASTING; POWDER METALLURGY
  • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
  • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
  • B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B22—CASTING; POWDER METALLURGY
  • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
  • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
  • B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
  • B22F1/102—Metallic powder coated with organic material
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B22—CASTING; POWDER METALLURGY
  • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
  • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
  • B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
  • B22F1/103—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material containing an organic binding agent comprising a mixture of, or obtained by reaction of, two or more components other than a solvent or a lubricating agent
• • 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
  • H01F1/44—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of magnetic liquids, e.g. ferrofluids
  • H01F1/442—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of magnetic liquids, e.g. ferrofluids the magnetic component being a metal or alloy, e.g. Fe
• • 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
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B22—CASTING; POWDER METALLURGY
  • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
  • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
  • B22F2998/10—Processes characterised by the sequence of their steps
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B22—CASTING; POWDER METALLURGY
  • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
  • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
• • C—CHEMISTRY; METALLURGY
  • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
  • C22C—ALLOYS
  • C22C2202/00—Physical properties
  • C22C2202/02—Magnetic

Definitions

• the present invention relates to a magnetic powder composite, an antenna, and an electronic device.
• Patent Document 1 describes a magnetic composite material that also functions in a high-frequency region.
• This magnetic composite material preferably has needle-shaped magnetic metal particles having an aspect ratio (major axis length / minor axis length) of 1.5 to 20 in a dielectric material such as polyarylene ether resin or polyethylene resin.
• a dielectric material such as polyarylene ether resin or polyethylene resin.
• Patent Document 2 describes a composite magnetic material that can be used for a small antenna that can be used in a wide band.
• This composite magnetic material is obtained by dispersing a composite magnetic material in an insulating material.
• the magnetic powder is a substantially spherical powder containing a soft magnetic metal, and has an average particle diameter D 50 of 0.1 to 3 ⁇ m, and a crystallite having an average crystallite diameter of 2 to 100 nm in the particles,
• Various resins are described as the insulating material ([0018] to [0021] of Patent Document 2).
• an antenna is manufactured by mixing magnetic powder, a thermoplastic PC / ABS resin, a solvent, and the like (see [0069]).
• tan ⁇ at a frequency of 2 GHz is less than 0.01, and that the volume ratio of the magnetic powder to the total volume is 2 to 50 vol%, so that the antenna can be miniaturized (see [0031] ] [0032].
• Patent Document 3 describes that the loss factor in the GHz band of an inductor, an antenna, or the like can be suppressed to a low level by using metal magnetic powder.
• a bonded magnet having heat resistance includes magnet powder, polyphenylene sulfide (PPS) resin, and polyamide (PA) resin, and the content ratio of the magnet powder in the magnetic composite is 79 to 94.5 wt%, It is described that the content ratio of the PPS resin is 5 to 20 wt% and the content ratio of the PA resin is 0.1 to 2 wt% (see [Claim 1] of Patent Document 4).
• magnetic compound As described above, there is a description of a magnetic composite containing metal magnetic powder and resin (also referred to as “magnetic compound”), but in a magnetic composite containing metal magnetic powder and resin, the metal magnetic powder is inorganic.
• the fine particles of the compound, and the resin is a polymer compound. That is, the metal magnetic powder and the resin have completely different chemical properties and physical properties. For this reason, it is difficult to predict the performance of the magnetic composite, and various trial and error studies are required as in the prior art.
• JP 2014-116332 A JP2011-096923A JP 2013-236021 A JP2013-077802A
• Patent Documents 1 to 4 disclose magnetic compounds having a high content ratio of magnetic powder.
• the content of the metal magnetic powder in the magnetic compound Sufficient high-frequency characteristics can be obtained even if the value is reduced to some extent.
• Patent Document 4 describes that other unexpected effects may occur during kneading and molding because the wettability between the PPS resin and the magnetic powder is poor (Patent Document 4 [[ [0008] [0035]). ). In the high frequency range, many resins with low dielectric loss can be seen, but it is difficult to obtain a magnetic compound with low dielectric loss even when kneading metal magnetic powder and resin to simply take good points. It was confirmed.
• the problem to be solved is to provide a metal magnetic powder that disperses well in a resin with a low dielectric loss, thereby providing a magnetic compound with a low dielectric loss, and thus an antenna formed from the magnetic compound and an electronic device incorporating the antenna.
• an antenna is formed from a resin in which metal magnetic powder is mixed with a resin, the antenna itself can be reduced due to the wavelength shortening effect, and thus downsizing of portable devices and smartphones. Can contribute.
• Patent Document 1 magnetic compound materials used for antennas and the like have been limited to investigations related to metal materials even if they are configured to be mixed with resin.
• the present inventor described above how to improve the familiarity with the resin to which the metal magnetic powder is mixed, instead of the metal magnetic powder alone that can be mixed with the resin and express the characteristics. We came up with a technological idea that there was a clue that could solve this problem.
• the first aspect of the present invention is: Metal magnetic powder, A magnetic powder composite comprising one or more selected from carboxylic acid or anhydride, aromatic carboxylic acid ester, and derivatives thereof, To a thermoplastic resin having a tan ⁇ at 1 MHz specified in IEC 60250 or JISC2138: 2007 of 0.05 or less with respect to 100 parts by mass of the metal magnetic powder, the carboxylic acid or its anhydride, an aromatic carboxylic acid ester, And 30% by volume of a magnetic powder composite prepared by adding 5 parts by mass of one or more selected from those derivatives, the real part ⁇ ′ of the permeability is 1.45 or more at a measurement frequency of 2 GHz. Tan ⁇ is 0.1 or less, and tan ⁇ is 0.05 or less.
• the second aspect of the present invention is:
• the said thermoplastic resin is a magnetic powder composite_body
• the third aspect of the present invention is: Metal magnetic powder, A magnetic powder composite comprising one or more selected from carboxylic acid or anhydride, aromatic carboxylic acid ester, and derivatives thereof, A material containing at least one selected from SPS, m-PPE, and PPS, and 100 parts by mass of the metal magnetic powder, the carboxylic acid or its anhydride, an aromatic carboxylic acid ester, and derivatives thereof
• 30% by volume of a magnetic powder composite prepared by adding one or more 5 parts by mass selected from the above is included, at a measurement frequency of 2 GHz, the real part ⁇ ′ of the magnetic permeability is 1.45 or more and tan ⁇ is 0. .1 or less, tan ⁇ is a magnetic powder composite having a property of showing a value of 0.05 or less.
• the fourth aspect of the present invention is: In the invention described in the first to third aspects,
• the carboxylic acid is a magnetic powder composite that is at least one selected from aromatic carboxylic acids, unsaturated carboxylic acids, and dicarboxylic acids.
• the magnetic powder composite has 4 or more and 30 or less carbon atoms constituting any of the carboxylic acid or its anhydride, aromatic carboxylic acid ester, and derivatives thereof.
• the sixth aspect of the present invention is: In the invention according to any one of the first to fifth aspects,
• the carboxylic acid or its anhydride, aromatic carboxylic acid ester, and derivatives thereof are phthalic acid, phthalic anhydride, maleic acid, maleic anhydride, succinic acid, succinic anhydride, malonic acid, fumaric acid, glutaric acid
• a magnetic powder composite which is at least one selected from azelaic acid, sebacic acid, benzoic acid, dimethyl phthalate and derivatives thereof.
• the seventh aspect of the present invention is The magnetic powder composite according to any one of the first to fifth aspects; A magnetic compound containing at least one resin selected from SPS and m-PPE.
• the eighth aspect of the present invention is Examples of the carboxylic acid or anhydride, aromatic carboxylic acid ester, and derivatives thereof include maleic acid, maleic anhydride, succinic acid, succinic anhydride, malonic acid, fumaric acid, glutaric acid, azelaic acid, sebacic acid, benzoic acid
• the magnetic powder composite according to the sixth aspect which comprises at least one selected from acids and derivatives thereof; A magnetic compound containing PPS resin.
• the ninth aspect of the present invention provides An antenna comprising the magnetic powder composite according to any one of the first to sixth.
• the tenth aspect of the present invention provides An electronic apparatus comprising an antenna constituted by the magnetic powder composite according to any one of the first to sixth.
• the eleventh aspect of the present invention is Metal magnetic powder, This is a method for producing a magnetic powder composite in which a magnetic powder composite is produced by mixing a carboxylic acid or an anhydride thereof, an aromatic carboxylic acid ester, and a derivative thereof.
• the twelfth aspect of the present invention provides Metal magnetic powder, In the step of mixing a carboxylic acid or its anhydride, an aromatic carboxylic acid ester, and a derivative thereof, a magnetic powder composite is produced by interposing a solution having a boiling point at 1 atm of 100 ° C. or less.
• the method for producing a magnetic powder composite according to the eleventh aspect is described in detail below.
• a magnetic powder composite that is well dispersed in a resin having a low dielectric loss, a magnetic compound having a low dielectric loss, and thus an antenna formed from the magnetic compound, and the antenna are incorporated.
• Electronic equipment can be provided.
• Magnetic powder composite for composing magnetic compounds > 1-1.
• Coating and magnetic powder composite ⁇ 2.
• “to” refers to a value that is greater than or equal to a predetermined value and less than or equal to a predetermined value.
• Magnetic powder composite for constituting magnetic compound includes a metal magnetic powder, a carboxylic acid, an anhydride produced by dehydration of a plurality of carboxylic acids, or an aromatic carboxylic acid. And one or more coatings selected from esters and their derivatives. Each configuration will be described below.
• Metal Magnetic Powder An example of the metal magnetic powder in the present embodiment has the following configuration.
• a magnetic powder, a particle size, and the like that are appropriately designed may be used.
• the magnetic permeability and dielectric constant of the magnetic compound can be set by saturation magnetization ( ⁇ s).
• the particle size, shape, BET (specific surface area), and TAP (tap) density may be adjusted as coercive force (Hc), squareness ratio (SQ), etc., and powder characteristics.
• the metal magnetic powder in the present embodiment includes Fe (iron), Fe and Co (cobalt), rare earth elements (including Y (yttrium), and so on), Al (aluminum), Si (silicon).
• Al etc. Mg (magnesium) (hereinafter referred to as “Al etc.”).
• the amount of rare earth elements is small, the axial ratio becomes large, and a metal powder with further reduced loss can be obtained, but the magnetic permeability is reduced.
• the amount of rare earth elements is large, the axial ratio is small and the loss is slightly increased, but the permeability is increased as compared with the case where the amount of rare earth elements is small.
• the metal magnetic powder by setting an appropriate rare earth content in the metal magnetic powder, it has lower loss and higher magnetic permeability. As a result, a metal magnetic powder that can be used in a wide range from kHz to GHz can be obtained.
• the specific content range of elements suitable for maintaining the balance of characteristics is 0 at% (preferably over 0 at%) to 10 at% in terms of rare earth element content relative to the total of Fe and Co. %, Preferably more than 0 at% and not more than 5 at%. Further, as the rare earth element species to be used, Y and La are preferable.
• the Co content is 0 to 60 at% in the atomic ratio of Co to Fe (hereinafter referred to as “Co / Fe atomic ratio”). More preferably, the Co / Fe atomic ratio is 5 to 55 at%, more preferably 10 to 50 at%. In such a Co / Fe atomic ratio range, the metal magnetic powder has a high saturation magnetization and a stable magnetic property is easily obtained.
• Al etc. also has a sintering suppression effect, and can suppress the coarsening of the metal magnetic powder particles due to sintering during heat treatment.
• Al or the like is treated as one of “sintering suppression elements”.
• Al or the like is a nonmagnetic component, it is preferably contained in a range that can ensure the magnetic properties of the metal magnetic powder.
• the content of Al or the like with respect to the total of Fe and Co is preferably 1 at% to 20 at%, more preferably 3 at% to 18 at%, and even more preferably 5 at% to 15 at%.
• the metal magnetic powder in the present embodiment preferably has a core / shell structure composed of a core made of a metal component and a shell mainly made of an oxide component. Whether or not it has a core / shell structure can be confirmed by, for example, a TEM photograph, and the composition analysis adopts methods such as ICP emission analysis, ESCA (aka XPS), TEM-EDX, SIMS, etc. can do.
• the average primary particle diameter of a metal magnetic powder is a nanoparticle of 10 nm or more and 500 nm or less (preferably 100 nm or less).
• a metal magnetic powder having a micro-level ( ⁇ m) size can be used, but a smaller particle size is desirable from the viewpoint of improving communication characteristics and downsizing the device.
• the blending may be adjusted so that the content of the metal magnetic powder is 50% by volume or less, preferably 40% by volume or less, more preferably 35% by volume or less with respect to a predetermined resin (described later). This is because the elastic modulus can be improved without impairing the bending strength of the resin while obtaining desired excellent communication characteristics.
• the coating in the present embodiment is formed on the surface of the metal magnetic powder by the surface treatment process described later, and becomes a magnetic powder composite. Presumably, the coating is considered to adhere to at least a part of the surface of the metal magnetic powder to form a magnetic powder composite.
• the said coating is 1 or more types selected from the carboxylic acid or the anhydride produced
• derivative refers to a compound that has been modified to such an extent that it does not significantly change the structure and properties of the matrix, such as the introduction of a functional group, oxidation, reduction, or atom replacement. The concept also includes those in which the terminal is substituted with an alkali metal and made soluble.
• carboxylic acids having a molecular weight of 500 or less are preferable to polymers having a molecular weight of tens of thousands such as resins. Further, those having 4 to 30 carbon atoms are preferred.
• carboxylic acid or anhydride thereof aromatic carboxylic acid ester, and derivatives thereof
• phthalic acid, phthalic anhydride, maleic acid, maleic anhydride, succinic acid, succinic anhydride, malonic acid It is preferably fumaric acid, glutaric acid, azelaic acid, sebacic acid, benzoic acid, dimethyl phthalate, and derivatives thereof, more preferably phthalic acid, phthalic anhydride, maleic acid, maleic anhydride, succinic acid, Those having a structure having 4 to 30 carbon atoms with succinic anhydride, malonic acid, fumaric acid, glutaric acid, azelaic acid, sebacic acid, benzoic acid and dimethyl phthalate as the main skeleton are preferred.
• carboxylic acids or their derivatives are not necessarily used alone, and do not prevent the use of a plurality of carboxylic acids.
• anhydride refers to a compound (relation between phthalic acid and phthalic anhydride) formed by removing water molecules from a compound by heating or the like (intramolecular dehydration), and two molecules of oxo acid. Also includes a compound obtained by dehydration condensation (relation between benzoic acid and benzoic anhydride).
• the carbon measurement value in the high frequency combustion method is 0.1% by mass or more and 10% by mass or less in the magnetic powder composite. It is preferable.
• the resin suitable in this embodiment is a thermoplastic resin having a tan ⁇ of 0.05 or less at 1 MHz specified in IEC60250 or JISC2138: 2007.
• the effect of this embodiment can be produced by using the resin.
• the use of a thermoplastic resin having an aromatic ring is preferable because tan ⁇ is good, and is particularly selected from SPS (syndiotactic polystyrene), PPS (polyphenylene sulfide), and m-PPE (modified polyphenylene ether). It is preferable to use one or more.
• one or more selected from PPS, SPS, and m-PPE are employed as the resin, and the resin and the magnetic powder composite according to the present invention are kneaded to form the magnetic according to the present invention. It is possible to produce a compound.
• the magnetic properties in the high frequency (2 GHz) region of the molded body given by the magnetic compound (composition of metal magnetic powder in the composite: equivalent to 30% by volume) according to the present invention are as follows: the real part ⁇ ′ of the complex relative permeability is 1. It is preferably 450 or more, preferably 1.50 or more, more preferably 1.70 or more.
• a magnetic compound having such characteristics is extremely useful for the construction of an antenna that can exhibit a sufficient size reduction effect due to its high magnetic permeability and has a small return loss.
• the magnetic powder composite is added to the thermoplastic resin or one or more resins selected from the PPS, SPS, and m-PPE.
• Magnetic powder prepared by adding 5 parts by mass of one or more selected from the carboxylic acid or anhydride, aromatic carboxylic acid ester, and derivatives thereof to 100 parts by mass of the metal magnetic powder as a body
• tan ⁇ is 0.10 or less, more preferably 0.05 or less, and more preferably 0.02 or less at a measurement frequency of 2 GHz. It is good to be. Further, tan ⁇ should be 0.10 or less, more preferably 0.05 or less, and still more preferably 0.02 or less.
• Step 2 various preparations related to the production of the magnetic compound are performed.
• various raw materials such as the above-described metal magnetic powder, raw materials for the covering, and a resin to be mixed are prepared.
• Coating process surface treatment
• a predetermined organic compound one or more selected from carboxylic acid, carboxylic anhydride, aromatic carboxylic acid ester and derivatives thereof
• carboxylic acids a carboxylic acid having a molecular weight of 500 or less is preferable to a polymer having a molecular weight of tens of thousands such as a resin. Further, the carbon number is preferably 4 to 30.
• carboxylic acids, carboxylic acid anhydrides, aromatic carboxylic acid esters, and derivatives thereof do not necessarily need to be composed of only one kind, and plural kinds of carboxylic acids, carboxylic acid anhydrides, aromatic carboxylic acid esters, and It does not prevent the use of these derivatives.
• the carbon content of the organic compound is 0.1% by mass or more because the magnetic powder composite can be suitably dispersed in the resin.
• the carbon content is 10% by mass or less, the nonmagnetic component does not become excessive, and the magnetic permeability when the magnetic powder composite or the magnetic compound formed thereafter is not lowered is preferable.
• the addition amount of the organic compound in the magnetic powder composite is 2 to 15, more preferably 2.5 to 10, and more preferably 5 to 10 with respect to the metal magnetic powder 100 in mass ratio.
• the mass ratio is 2 or more, the metal magnetic powder and the resin become compatible, so that the property stability of the product when produced is improved.
• the nonmagnetic component in the metal magnetic powder becomes an appropriate amount, and a decrease in the magnetic properties of the magnetic powder composite itself composed of the metal magnetic powder coated with the coating can be suppressed.
• the high frequency characteristics when the magnetic powder composite is mixed with the resin to form a magnetic compound can be kept relatively high, and the characteristics of the antenna finally formed can be kept relatively high as well. it can.
• a predetermined solvent a liquid to be added to improve the familiarity between the powder and the coating
• a solvent having a boiling point of 100 ° C. or less at 1 atm is added, the familiarity between the metal magnetic powder and the carboxylic acid or anhydride, aromatic carboxylic acid ester, and derivatives thereof can be improved.
• the added solvent can be removed even with slight heating.
• the predetermined solvent various alcohols, hydrocarbon solvents, ketones, ethers and the like can be used, and the above-mentioned carboxylic acid or its anhydride, aromatic carboxylic acid ester, and derivatives organic compounds thereof are not necessarily completely. It does not need to be soluble. Specific examples include ethanol, methanol, propanol, IPA, hexane, acetone, butanone, but are not limited thereto. A particularly preferred embodiment is preferably alcohols, particularly ethanol for ease of handling. Therefore, in order to obtain a dried magnetic powder composite, a method is adopted in which a metal magnetic powder is added to the above organic compound and the solvent added, the metal magnetic powder is impregnated in the solvent, and then the solvent is removed. This is convenient.
• a method is adopted in which a metal magnetic powder is added to the above organic compound solution, and the mixture is agitated with a rotating and revolving combined stirrer or stirred while applying a shearing force to form a paste. May be.
• the organic compound and the metal magnetic powder are mixed so that they are well-adapted, so that the organic compound is easily adsorbed on the surface of the metal magnetic powder, and thus a covering is easily formed. . That is, there is no problem as long as the organic substance added to the metal magnetic powder spreads uniformly.
• a mixer or the like may be used for removing the solvent and drying while kneading. It is important to leave the organic compound on the surface of the metal magnetic powder after the removal and drying.
• a dispersion having a high shearing force A kneader may be used, and a method of dispersing the metal magnetic powder in the solvent while applying a strong shearing force to the solvent may be employed.
• T.K. of PRIMIX Co., Ltd. known as a turbine-stator type stirrer is used as a disperser having a strong shearing force used when adopting a method of drying into a powder state after producing the paste.
• K. Examples include Homomixer (registered trademark), Ultra-Turrax (registered trademark) of IKA, and the like.
• the strength of the shearing force described above can be evaluated by the peripheral speed of the stirring blade if the device has the stirring blade.
• the “strong shearing force” refers to a blade peripheral speed of 3.0 (m / s) or more, preferably 5.0 (m / s) or more.
• the blade peripheral speed is equal to or higher than the above value, the shearing force is moderately high, the pasting time can be shortened, and the production efficiency is moderately good.
• the blade peripheral speed can be calculated by the following equation: Circumference ratio x Turbine blade diameter (m) x Stirring rotation speed (rotation speed) per second. For example, if the turbine blade diameter is 3.0 cm (0.03 m) and the stirring rotation speed is 8000 rpm, the rotation speed per second is 133.3 (rps), and the blade peripheral speed is 12.57 (m / S).
• the obtained paste-like processed product may be dried to remove the solvent.
• the paste can be spread on the vat and dried by setting the temperature to be equal to or higher than the drying temperature of the solvent and lower than the decomposition temperature of the coating substance.
• the solvent is preferably dried in nitrogen under an inert atmosphere in terms of cost.
• a method may be employed in which drying is performed after removing a certain amount of solvent by filtration.
• drying time can also be shortened.
• cover in order to confirm whether the said coating
• the metal magnetic powder When performing such a treatment, it is preferable to carry out the treatment in an inert atmosphere for the purpose of suppressing deterioration of characteristics due to oxidation of the metal magnetic powder. Furthermore, it is more preferable to perform an operation of passing an inert gas (nitrogen in terms of cost) through a liquid once mixed with a solvent and an organic compound. After the inside of the processing vessel is replaced with an inert gas, the metal magnetic powder is added so as not to oxidize, and a solvent, an organic compound, and the metal magnetic powder are mixed to prepare a mixture. Drying can be performed by setting the temperature to be equal to or higher than the drying temperature and lower than the decomposition temperature of the coating substance. In order to dry in a shorter time, it is preferable that the mixer is operated and dried while rolling the mixture.
• an inert gas nitrogen in terms of cost
• coarse particles are preferably removed using a classifier or a sieve. This is because by removing large coarse particles, it is possible to avoid a situation in which force is applied to a portion where coarse particles are present and mechanical characteristics deteriorate when an antenna is manufactured.
• classifying using a sieve it is appropriate to use one having an opening of 500 mesh or less.
• BET specific surface area A BET specific surface area is calculated
• the means for producing the magnetic compound there are no particular restrictions on the means for producing the magnetic compound.
• the kneading strength and the like may be adjusted using a commercially available kneader.
• a method of heating a mixture containing a resin, a metal magnetic powder, and the above organic compound to produce a magnetic compound may be employed, or a method of adding a magnetic powder composite to a melted resin may be employed. It doesn't matter.
• the melting temperature of the resin is usually higher than the melting temperature of the resin, and is set below the decomposition temperature when the decomposability of the resin is high.
• a fiber state glass fiber which is a fiber state glass fiber, carbon fiber, graphite fiber, aramid fiber, vinylon fiber, polyamide fiber, polyester Fiber, hemp fiber, kenaf fiber, bamboo fiber, steel fiber, cotton, rayon, aluminum fiber, carbon nanofiber, carbon nanotube, cotton fibril, silicon nitride whisker, alumina whisker, silicon carbide whisker, nickel whisker, plate-like talc , Kaolin clay, mica, glass flake, aragonite, calcium sulfate, aluminum hydroxide, organic montmorillonite, swelling synthetic mica, graphite, granular calcium carbonate, silica, glass beads, titanium oxide, zinc oxide, wollastonite, Bamiki Light can be added Shirasu balloons, glass balloons, nano titanium oxide, nano silica, things like carbon black.
• a substance that suppresses deterioration over time can be added within a range in which the characteristics
• the high frequency characteristics of the obtained magnetic compound molded body that is, the interval of 0.5 to 5 GHz, the measurement width is in increments of 0.05 GHz
• the real part of the magnetic permeability ( ⁇ ′), the imaginary number of the magnetic permeability Part ( ⁇ ′′), real part of dielectric constant ( ⁇ ′), and imaginary part of dielectric constant ( ⁇ ′′) were measured to confirm high frequency characteristics.
• tan ⁇ ⁇ ′′ / ⁇ ′
• Metal magnetic particles, coatings, magnetic powder composites and resins Metal magnetic particles, coatings, magnetic powder composites and resins
• the main elements and compounds have been described in detail regarding the metal magnetic particles, the covering, the magnetic powder composite, and the resin.
• the metal magnetic particles, the covering, the magnetic powder composite, and the resin may contain materials other than the elements and compounds listed above.
• a magnetic compound composed of the magnetic powder composite and a specific resin obtained in the present embodiment can be used for an antenna, an inductor, and a radio wave shielding material.
• Such an electronic communication device includes, for example, a portion that functions as an electronic communication device based on the radio wave received by the antenna in the present embodiment, and a control unit that controls the portion based on the received radio wave. Things.
• the electronic communication device in the present embodiment is preferably a communication device having a communication function because it includes an antenna.
• an electronic device that does not have a communication function such as a telephone call may be used as long as it is an electronic device that receives radio waves from an antenna and performs its function.
• Tables 1 to 5 show the conditions and measurement results in each example given in this item.
• Table 1 describes the raw materials of the samples according to Examples 1 to 20 and Comparative Examples 1 to 6.
• Table 2 describes the magnetic properties and mechanical properties of the samples according to Examples 1 to 20 and Comparative Examples 1 to 6.
• Table 3 describes the high-frequency characteristics (750 MHz to 1 GHz, 2 GHz) of the samples according to Examples 1 to 20 and Comparative Examples 1 to 6.
• Table 4 describes the high frequency characteristics (800 MHz, 1.5 GHz) of the samples according to Examples 1 to 20 and Comparative Examples 1 to 6.
• Table 5 describes the high frequency characteristics (2.5 GHz, 3.0 GHz) of the samples according to Examples 1 to 20 and Comparative Examples 1 to 6.
• the blanks in each table are items that were not measured or could not be measured.
• Example 1 a small sample was prepared.
• the metal magnetic powder DOWA Electronics Co., Ltd.: iron - cobalt metal particles, major axis length: 40nm, BET: 37.3m 2 /g, ⁇ s:179.3Am 2 / kg, the carbon content (high-frequency combustion method) : 0.01% by mass) with a 500 mesh sieve, phthalic acid (special grade reagent manufactured by Wako Pure Chemical Industries) is added to the metal magnetic powder (50 g) under the sieve and 5% (2.5 g) of the magnetic powder. ), 30% by weight (15 g) of ethanol was added to the magnetic powder and mixed for 5 minutes in an agate mortar.
• the metal magnetic powder DOWA Electronics Co., Ltd.: iron - cobalt metal particles, major axis length: 40nm, BET: 37.3m 2 /g, ⁇ s:179.3Am 2 / kg, the carbon content (high-frequency combustion method) : 0.01% by mass
• phthalic acid special grade
• the true density of the obtained magnetic powder composite was determined by a gas phase (He gas) substitution method to be 5.58 g / cm 3 .
• the obtained true density value was used for calculation of the blending ratio for making the content of the magnetic powder composite in the compound a desired ratio.
• the obtained magnetic compound was put into an injection molding machine, which is an optional device of a small kneader, under conditions of a cylinder temperature of 300 ° C. and a mold temperature of 130 ° C., and a molded body for bending test (ISO178 standard size: 80 mm ⁇ 10 mm ⁇ 4mm), and using a digital force gauge (manufactured by Imada Co., Ltd., ZTS-500N), the distance between fulcrums was set to 16 mm, the bending strength was measured, the bending displacement was calculated, and the elastic modulus (MPa) was measured. .
• a digital force gauge manufactured by Imada Co., Ltd., ZTS-500N
• 0.2 g of the magnetic compound was put into a donut-shaped jig having a diameter of 6 mm, and then heated at 300 ° C. for 20 minutes with a small hot press machine (manufactured by ASONE). In this way, after the resin in the magnetic compound is melted, it is molded and cooled into a toroidal shaped molded body having an outer diameter of 7 mm and an inner diameter of 3 mm while applying pressure.
• the high frequency characteristics were measured by the method described in the embodiment.
• Example 2 This example was the same as Example 1 except that the treatment agent added in Example 1 was maleic anhydride.
• Example 3> This example was the same as Example 1 except that the treatment agent added in Example 1 was maleic acid.
• Example 4 This example was the same as Example 1 except that the treatment agent added in Example 1 was dimethyl phthalate.
• Example 5> This example was the same as Example 1 except that the treatment agent added in Example 1 was succinic acid.
• Example 6> This example was the same as Example 1 except that the treatment agent added in Example 1 was succinic anhydride.
• Example 7 This example was the same as Example 1 except that the treatment agent added in Example 1 was phthalic anhydride.
• Example 8> This example was the same as Example 1 except that the treatment agent added in Example 1 was benzoic acid.
• Example 9 This example was the same as Example 1 except that the treatment agent added in Example 1 was malonic acid.
• Example 10> This example was the same as Example 1 except that the treating agent added in Example 1 was fumaric acid.
• Example 11 This example was the same as Example 1 except that the treatment agent added in Example 1 was glutaric acid.
• Example 12 This example was the same as Example 1 except that the treatment agent added in Example 1 was azelaic acid.
• Example 13> This example was the same as Example 1 except that the treatment agent added in Example 1 was sebacic acid.
• Example 14 a medium amount sample was produced.
• ethanol special grade reagent manufactured by Wako Pure Chemical Industries, Ltd.
• phthalic acid special grade reagent manufactured by Wako Pure Chemical Industries, Ltd.
• phthalic acid was dissolved in ethanol.
• the metal magnetic powder DOWA Electronics Co., Ltd.: iron - cobalt metal particles, major axis length: 40nm, BET: 37.3m 2 /g, ⁇ s:179.3Am 2 / kg
• TK homomixer Mark II manufactured by PRIMIX Corporation
• the obtained paste was spread on an aluminum vat, heated for 1 hour at around the volatilization temperature of ethanol (78 ° C), then heated to 120 ° C and heated for 1.5 hours, ethanol was removed from the paste, phthalic acid and metal Agglomerates mixed with magnetic powder were obtained.
• the obtained agglomerate was passed through a 500 mesh screen to remove coarse particles to obtain a magnetic powder composite according to this example.
• the resulting magnetic powder composites, BET: 34.9m 2 /g, ⁇ s:173.5Am 2 / kg, the carbon content (high-frequency combustion method): 2.82 were those having a mass% of properties.
• the true density of the magnetic powder composite is obtained by a gas phase (He gas) substitution method, and the blended ratio for making the obtained true density value a desired ratio of the content of the magnetic powder composite in the compound. Used to calculate Thereafter, evaluation was performed in the same manner as in Example 1.
• He gas gas phase
• Example 15 Example 14 was carried out except that the resin was changed to DURAFIDE (registered trademark) 1130A64 (PPS / polyphenylene sulfide manufactured by Polyplastics Co., Ltd.) having a specific gravity of 1.57 g / cm 3 containing 30% glass fiber. And so on.
• DURAFIDE registered trademark
• 1130A64 PPS / polyphenylene sulfide manufactured by Polyplastics Co., Ltd.
• Example 16 a magnetic powder composite having a volume filling rate of 20% by volume at the time of forming a molded body and XAREC (registered trademark) SP105 (SPS / Idemitsu Kosan Co., Ltd., SyndioTac, having a specific gravity of 1.18 g / cm 3 ).
• 11.5 g of tic polystyrene was weighed in nitrogen, placed in a No. 5 standard bottle, and capped. After lightly shaking by hand, the mixture was kneaded for 10 minutes with a small kneader (DSM Xplore (registered trademark) MC15, manufactured by Xplo Instruments) at a set temperature of 300 ° C. and a kneading stirring speed of 100 rpm. Resin and magnetic powder were added) to prepare a kneaded product, that is, a magnetic compound. The remainder was evaluated in the same manner as in Example 1.
• DSM Xplore registered trademark
• MC15
• Example 17 In this example, the same procedure as in Example 16 was performed except that the addition amount of the magnetic powder composite and SPS was adjusted so that the volume filling rate of the magnetic powder composite was equivalent to 30% by volume.
• Example 18 In this example, the same procedure as in Example 16 was performed, except that the addition amount of the magnetic powder composite and SPS was adjusted so that the volume filling rate of the magnetic powder composite corresponds to 40% by volume.
• Example 19 In this example, the same procedure as in Example 16 was performed except that the resin was changed to Zylon (registered trademark) AH-40 (PPE / modified polyphenylene ether manufactured by Asahi Kasei Chemicals Corporation) having a specific gravity of 1.06 g / cm 3 .
• Zylon registered trademark
• AH-40 PPE / modified polyphenylene ether manufactured by Asahi Kasei Chemicals Corporation
• Example 20 In this example, the resin was changed to Zylon (registered trademark) GH-30 (PPE / modified polyphenylene ether manufactured by Asahi Kasei Chemicals Corporation) having a specific gravity of 1.31 g / cm 3 containing 30% glass fiber. Same as 16.
• Zylon registered trademark
• GH-30 PPE / modified polyphenylene ether manufactured by Asahi Kasei Chemicals Corporation
• Example 1 metal magnetic particles not surface-treated with phthalic acid in Example 1 were used. Furthermore, an epoxy resin (one-pack type epoxy resin, manufactured by Tesque Co., Ltd.), which is not a thermoplastic resin but a thermosetting resin, is weighed so that the metal magnetic powder is 30% by mass. Using a defoaming mixer (V-mini300), the metal magnetic powder was dispersed in an epoxy resin to form a paste. This paste was dried on a hot plate at 60 ° C. for 2 hours to obtain a metal magnetic powder-resin composite. This composite is pulverized to prepare a composite powder. 0.2 g of this composite powder is placed in a donut-shaped container, and a load of 1 t is applied by a hand press machine. A 3 mm toroidal shaped body was obtained. Thereafter, evaluation was performed in the same manner as in Example 1.
• an epoxy resin one-pack type epoxy resin, manufactured by Tesque Co., Ltd.
• V-mini300 defoaming mixer
• Example 3 This example was the same as Example 14 except that the metal magnetic powder was not surface-treated with phthalic acid. In this example, when the kneaded material was produced, the metal magnetic powder ignited and smoke was generated at the stage when the kneaded material was taken out into the atmosphere, and the kneaded material could not be produced in the first place.
• Example 4 This example was the same as Example 17 except that the surface of the metal magnetic powder was not treated with phthalic acid. In this example, when the kneaded material was produced, the metal magnetic powder ignited and smoke was generated at the stage when the kneaded material was taken out into the atmosphere, and the kneaded material could not be produced in the first place.
• Example 5 This example was the same as Example 19 except that the metal magnetic powder was not surface-treated with phthalic acid. In this example, when the kneaded material was produced, the metal magnetic powder ignited and smoke was generated at the stage when the kneaded material was taken out into the atmosphere, and the kneaded material could not be produced in the first place.
• Example 6 it was confirmed whether the same effect was seen in the magnetic powder composite by using a mixed resin of thermoplastic resin and aromatic nylon which is an existing technology.
• the metal magnetic powder was not surface-treated with phthalic acid, and the resin was DURAFIDE (registered trademark) (PPS / polyphenylene sulfide resin A0220A9 manufactured by Polyplastics Co., Ltd.) and aromatic Nylon 6T Vestamide (registered trademark) (HTplus M1000 manufactured by Daicel-Evonik Co., Ltd.) was mixed in the same manner.
• DURAFIDE registered trademark
• aromatic Nylon 6T Vestamide registered trademark
• HTplus M1000 manufactured by Daicel-Evonik Co., Ltd.

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