WO2019159800A1 - 複合粒子、粉末、樹脂組成物および成形体 - Google Patents

複合粒子、粉末、樹脂組成物および成形体 Download PDF

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WO2019159800A1
WO2019159800A1 PCT/JP2019/004304 JP2019004304W WO2019159800A1 WO 2019159800 A1 WO2019159800 A1 WO 2019159800A1 JP 2019004304 W JP2019004304 W JP 2019004304W WO 2019159800 A1 WO2019159800 A1 WO 2019159800A1
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Prior art keywords
particles
powder
ferrite
particle
mass
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PCT/JP2019/004304
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English (en)
French (fr)
Japanese (ja)
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康二 安賀
一隆 石井
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パウダーテック株式会社
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Priority to JP2020500438A priority Critical patent/JPWO2019159800A1/ja
Priority to TW108104592A priority patent/TW201936545A/zh
Publication of WO2019159800A1 publication Critical patent/WO2019159800A1/ja

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00—Compounds of iron
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81—Coating or impregnation
    • C04B41/85—Coating or impregnation with inorganic materials
    • C04B41/88—Metals
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/20—Conductive material dispersed in non-conductive organic material
    • H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
    • 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
    • H01F1/34—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 non-metallic substances, e.g. ferrites
    • 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
    • H01F1/34—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 non-metallic substances, e.g. ferrites
    • H01F1/36—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 non-metallic substances, e.g. ferrites in the form of particles
    • H01F1/37—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 non-metallic substances, e.g. ferrites in the form of particles in a bonding agent
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K9/00—Screening of apparatus or components against electric or magnetic fields

Definitions

  • the present invention relates to composite particles, powder, a resin composition, and a molded body.
  • the electronic components By being mounted in a high density in the housing, the electronic components are close to each other and are easily affected by electromagnetic noise generated from the electronic circuit, and the heat generated from the electronic components is difficult to escape. Therefore, an electronic component that operates at a higher temperature and a material that can suppress electromagnetic noise are desired. Furthermore, electric vehicles and hybrid vehicles are also being electrically equipped, and there is a need for noise suppression materials around parts that operate at high temperatures for a long time.
  • An object of the present invention is to provide composite particles and powder excellent in electromagnetic wave shielding properties, to provide a molded body excellent in electromagnetic wave shielding properties, and a resin composition that can be suitably used for producing the molded body. To provide things.
  • [9] [8] A resin composition comprising the powder according to [8] and a resin material.
  • [10] A molded article produced using a material comprising the powder according to [8] and a resin material.
  • the present invention it is possible to provide composite particles and powder excellent in electromagnetic wave shielding properties, to provide a molded body excellent in electromagnetic wave shielding properties, and a resin composition that can be suitably used for producing the molded body. Things can be provided.
  • FIG. 2 is a cross-sectional SEM image of the composite particles of Example 1.
  • FIG. It is a cross-sectional EDX mapping image (Ag) of the composite particle of Example 1. It is a graph which shows the representative example of the evaluation result of the electromagnetic wave shielding effect by KEC method.
  • the composite particle of the present invention includes a plate-like base particle made of ferrite and a coating layer made of a material containing at least one selected from the group consisting of Au, Ag, Pt, Ni and Pd. ing.
  • the powder of the present invention contains a plurality of the composite particles of the present invention.
  • the composite particle and powder excellent in the shielding property of electromagnetic waves can be provided.
  • Such an excellent effect can be obtained by providing the mother particles having excellent electromagnetic wave absorbability and the coating layer having excellent electromagnetic wave reflectivity so that they act synergistically.
  • the weight can be reduced as compared with the case where the particles composed only of the metal material as described above are used. Therefore, for example, it can be suitably applied to mobile terminals such as mobile phones, smartphones, and tablets.
  • the amount of expensive metal used can be suppressed, and the overall cost can be reduced.
  • the electromagnetic wave shielding property of the molded body can be made excellent. That is, the composite particles can be oriented in a specific direction (a direction along the surface of the molded body), and it becomes difficult to form a gap between the particles, and the electromagnetic wave shielding property can be improved. In addition, because it is coated with a highly conductive metal and has high orientation, the electrical orientation (volume resistance) in the orientation direction of the particles is low, and the electrical resistance (volume resistance) in the direction perpendicular to the orientation direction is high. It becomes easy.
  • the composite particles and powder can be adjusted to a color tone other than black. More specifically, by providing a coating layer composed of a material containing Au, the color tone of the composite particles and powder can be adjusted to gold. In addition, by providing a coating layer made of a material containing at least one selected from the group consisting of Ag, Pt, Ni, and Pd, the color tone of the composite particles and powder is suitably adjusted to a color tone of white to silver. be able to. Thereby, for example, not only can the color tone of the molded product containing composite particles and powder be suitably adjusted to a white to silver color tone, but also the molded product can contain a colorant (including providing a printing layer). Thereby, a molded object can be adjusted to a desired color tone.
  • the conductivity of the composite particles, powders, and compacts containing these can be made excellent.
  • a conductive path is selectively formed in a specific direction, and the resin molded body
  • the resistance can be anisotropic.
  • particles in a molded body produced using the powder of the present invention, particles (composite particles) can be suitably joined under relatively mild conditions. Thereby, the shielding property of electromagnetic waves and the low mechanical strength of the molded body can be compatible at a higher level.
  • the frequency characteristics of the magnetic permeability of the composite particles can be controlled by controlling the thickness of the coating layer made of a material containing a highly conductive noble metal.
  • particles that do not have a coating layer as described above cannot sufficiently obtain the effect of electromagnetic wave reflection as described above, and have sufficiently excellent electromagnetic wave shielding properties as a whole. It can not be.
  • the color tone of the particles is black with low brightness, it is difficult to adjust the color tone of the molded body containing the powder.
  • the conductivity of the particles, powders, and compacts containing them cannot be made sufficiently excellent.
  • the mother particles when used for the production of a molded product (resin molded product), the molded product has a sufficient shielding property against electromagnetic waves (when added at the same weight). It becomes difficult to make it excellent. Further, if the content of the mother particles is increased in order to obtain the same level of electromagnetic wave shielding properties, problems such as an increase in the weight of the molded product occur.
  • the plate shape includes a flat plate shape and a curved plate shape.
  • the mother particles are composed of ferrite having a plate shape.
  • the mother particles may include, for example, hard ferrite, but are preferably composed of soft ferrite.
  • the magnetic permeability can be easily controlled in a wide frequency range (for example, 1 MHz to 1 GHz).
  • the composition of the ferrite constituting the mother particle is not particularly limited.
  • Mn—Zn ferrite, Ni—Zn ferrite, Ni—Zn—Cu ferrite, Ba ferrite, Sr ferrite, Mn ferrite, Mn -Mg based ferrite or the like can be used.
  • Ni—Zn ferrite for example, Fe is 45% by mass or more and 52% by mass or less, Ni is 5% by mass or more and 25% by mass or less, and Zn is 1.0% by mass or more and 25% by mass or less. What is contained with the content rate of can be used.
  • Ni—Zn—Cu based ferrite include Fe of 45 mass% to 52 mass%, Ni of 5 mass% to 25 mass%, Zn of 1.0 mass% to 25 mass%, and Cu of 1%. What is contained with the content rate of the mass% or more and 6 mass% or less can be used.
  • the Sr-based ferrite for example, a ferrite containing Fe in a content of 61.0% by mass to 65.0% by mass and Sr in a content of 7.8% by mass to 9.0% by mass can be used.
  • the Mn-based ferrite for example, one containing Fe in a content of 50% by mass to 70% by mass and Mn in a content of 3.5% by mass to 20% by mass can be used.
  • the Mn—Mg ferrite for example, the Fe content is 43 mass% to 65 mass%, the Mn content is 10 mass% to 25 mass%, and the Mg content is 1 mass% to 6.0 mass%. What is contained with the content rate of the mass% or less can be used.
  • the ferrite of each series described above may contain a metal element (other metal element) that does not indicate the content rate.
  • the content rate of the said other metal element is 1.0 mass% or less, respectively.
  • the mother particles are preferably composed of Mn—Zn ferrite.
  • the mother particles are preferably composed of Mn—Zn ferrite.
  • the Mn—Zn-based ferrite may be ferrite containing Mn and Zn as constituent components, but Fe is 45 mass% to 65 mass%, Mn is 5 mass% to 20 mass%, and Zn is 0.8 mass%. It is preferable to have a composition containing at a content of not less than mass% and not more than 13 mass%. Further, it is more preferable that the composition contains Fe in a content of 45% by mass to 60% by mass, Mn in a content of 4% by mass to 18% by mass, and Zn in a content of 1% by mass to 10% by mass.
  • the Mn content is too low, depending on the Zn content, oxidation tends to proceed during the production of particles by approaching magnetite, and the desired magnetic properties may not be obtained.
  • the magnetization tends to be lowered, depending on the Zn content.
  • the magnetization tends to decrease although it depends on the Mn content.
  • the Curie point (also referred to as Curie temperature) of the ferrite constituting the mother particle is preferably 200 ° C. or higher and 500 ° C. or lower, and more preferably 220 ° C. or higher and 450 ° C. or lower.
  • the heat resistance of the composite particles and the molded body produced using the composite particles can be made excellent, and for example, it can be suitably applied to a molded body used in a high temperature environment.
  • the Curie temperature itself is not too high, there is no problem, but the Curie point of ferrite is determined by the composition, and the above ferrite composition usually does not exceed 500 ° C.
  • the Curie point is obtained as follows.
  • the above-mentioned Curie point is obtained from measurement of the change in magnetization of the ferrite powder due to temperature change using a vibrating sample magnetometer (VSM) (VSM-5 type manufactured by Toei Kogyo).
  • VSM vibrating sample magnetometer
  • the temperature at which the tangent of the curve crosses the line where the magnetization becomes 0 from the low temperature side immediately before the magnetization becomes 0 is defined as the Curie point.
  • the mother particles are plate-shaped, but it is particularly preferable that the following conditions (average plate diameter, average thickness, aspect ratio) are satisfied.
  • the average plate diameter (average length in the major axis direction) of the mother particles is preferably 10 ⁇ m or more and 2000 ⁇ m or less, more preferably 15 ⁇ m or more and 1000 ⁇ m or less, and further preferably 20 ⁇ m or more and 500 ⁇ m or less.
  • the aspect ratio of the mother particles can be made relatively large, the influence of the demagnetizing field generated by the ferrite particles themselves can be reduced, and the electromagnetic wave shielding ability can be further enhanced.
  • the adhesion between the particles in the main firing at the time of production is suppressed, the length (thickness) in the minor axis direction can be reduced, and plate-like particles having a desired thickness can be obtained more easily.
  • the average plate diameter (average length in the major axis direction) can be obtained as follows. That is, SEM photographs of particles to be measured are taken using FE-SEM (Field Emission-Scanning Electron Microscope), and the length (length in the long axis direction) is determined for each particle using the automatic particle analysis function attached to EDX. ). Of the measured particles, those that clearly show the thickness direction of the particles, those that are fixed while standing at the time of FE-SEM observation, and those that recognize a plurality of particles as one particle are excluded. The average value for the particles can be taken as the average plate diameter. As FE-SEM, SU-8020 manufactured by Hitachi High-Tech is used and photographed at an acceleration voltage of 15 KV and 200 times magnification. As EDX, X-MAX manufactured by Horiba is used, and image information is obtained from FE-SEM. Particle analysis is automatically performed over multiple fields of view while obtaining
  • the average thickness (average length in the minor axis direction) of the mother particles is preferably 0.5 ⁇ m or more and 100 ⁇ m or less, more preferably 1.0 ⁇ m or more and 50 ⁇ m or less, and 2.0 ⁇ m or more and 30 ⁇ m or less. More preferably.
  • the strength of the mother particles becomes sufficient, cracks during production can be more effectively suppressed, electromagnetic wave shielding ability can be further improved, and the composite particles of the present invention and molding including powder
  • a molded body having a smoother curved surface can be more suitably produced.
  • the average thickness (average length in the minor axis direction) is determined as follows. That is, first, 9 g of an aggregate of particles to be measured and 1 g of a powder resin are placed in a 50 cc glass bottle, mixed for 30 minutes in a ball mill, and the resulting mixture is placed in a 13 mm diameter die and pressure molded at a pressure of 30 MPa. . Thereafter, the molded body is embedded in a resin in a vertically standing state so that a cross section of the molded body can be seen, and polished with a polishing machine to obtain a thickness measurement sample.
  • the prepared thickness measurement sample is photographed with an FE-SEM at a magnification of 50 to 800 times, and the thickness (length in the minor axis direction) of the obtained particle is measured without the protrusion. To do. And the arithmetic average of the thickness of 100 particle
  • the FE-SEM was SU-8020 manufactured by Hitachi High-Tech Co., Ltd., and was photographed at an acceleration voltage of 15 KV.
  • As the powder resin Kynar 301F manufactured by Arkema was used.
  • the aspect ratio of the mother particles is preferably 4 or more and 1000 or less, more preferably 4 or more and 200 or less, and even more preferably 4 or more and 100 or less.
  • the influence of the demagnetizing field generated by the ferrite particles themselves can be reduced, the electromagnetic shielding performance can be further enhanced, and the electromagnetic shielding ability and the flexibility of the molded product when formed into a molded product can be obtained.
  • mother particles may be in the form of a plate, but are preferably indefinite.
  • indefinite shape means that one specific direction (thickness direction, short axis direction) is almost constant when the particle is three-dimensionally expressed, and the shape in the remaining plane direction is a specific circle or polygon. It means that the shape is not regular.
  • the perimeter of the particle is constituted by a plurality of combinations of arbitrary straight lines and arbitrary curves.
  • the shape factor SF-2 of the mother particles is preferably 125 or more and 300 or less, more preferably 138 or more and 290 or less, and further preferably 140 or more and 280 or less.
  • the shape factor SF-2 is an index representing the degree of irregularity. The closer the particle shape is to a sphere or circle, the closer to 100. On the other hand, when the shape factor SF-2 is large, the deviation of the perimeter of the particle from the envelope length increases, which means that the recessed portion of the perimeter increases.
  • the indefinite form means that SF-2 is 125 or more.
  • the shape factor SF-2 when producing a molded body containing composite particles, it is possible to more effectively suppress the formation of gaps (portions where electromagnetic waves easily pass) between the composite particles.
  • the electromagnetic wave shielding property can be further improved. It is also advantageous from the viewpoint of reducing the production cost of the composite particles.
  • the shape factor SF-2 is a value obtained by dividing a value obtained by squaring the projected peripheral length L of the particle by the projected area S of the particle and 4 ⁇ and multiplying by 100, and is calculated by the following equation: .
  • the shape factor SF-2 is obtained by the same measurement as that for measuring the average plate diameter. That is, an SEM photograph of particles to be measured is taken using FE-SEM, and the perimeter length and projected area are measured for each particle using an automatic particle analysis function attached to EDX. The shape factor SF-2 is calculated. Of the measured particles, those that clearly show the thickness direction of the particles, those that are fixed while standing at the time of FE-SEM observation, and those that recognize a plurality of particles as one particle are excluded. The average value for the particles may be the shape factor SF-2. As FE-SEM, SU-8020 manufactured by Hitachi High-Tech is used and photographed at an acceleration voltage of 15 KV and 200 times magnification. As EDX, X-MAX manufactured by Horiba is used, and image information is obtained from FE-SEM. Particle analysis is automatically performed over multiple fields of view while obtaining
  • the mother particle may have one or more protrusions on the surface (main surface).
  • the adhesion between the mother particles and the coating layer can be made excellent, and the effects of the present invention described in this specification can be obtained over a longer period of time and more stably.
  • the number of protrusions provided on one mother particle is not particularly limited, but is preferably 1 or more and 30 or less.
  • the height of the protrusion is preferably smaller than the thickness of the mother particle (thickness of the portion excluding the protrusion. In the present specification, the same applies to other described portions unless otherwise specified).
  • the height of the protrusion is preferably smaller than the thickness of the coating layer. Thereby, it can prevent more effectively that the part which is not coat
  • the conditions for the protrusions can be suitably adjusted according to, for example, the manufacturing conditions of the mother particles.
  • the protrusion is suitably formed by controlling the oxygen concentration in the main baking and heat treatment, or by using a substrate having a minute recess on the surface as the base material to which the liquid composition is applied. Can do.
  • mother particles of all the composite particles constituting the powder of the present invention may have protrusions, or only the mother particles of some of the composite particles may have protrusions.
  • the average surface roughness (Ra) of the mother particles is not particularly limited, but is preferably 0.01 ⁇ m to 3 ⁇ m, and more preferably 0.1 ⁇ m to 1.5 ⁇ m.
  • the average surface roughness (Ra) is determined as follows. The surface roughness was measured according to JIS B 0601-2001. Measurement was performed on 100 particles randomly selected using a 3D laser microscope LEXT OLS4000 manufactured by Olympus, the surface roughness was calculated from the unevenness of the obtained surface particles, and the average value of the surface roughness of each particle obtained was calculated. Used as the average surface roughness Ra.
  • the mother particle constituting the single composite particle may be composed of, for example, a single particle, or a joined body (including aggregates) of a plurality of fine particles.
  • the mother particle only needs to be made of a material containing ferrite, and may contain other components, for example.
  • the content of components other than ferrite in the mother particles is preferably 1.0% by mass or less, more preferably 0.7% by mass or less, and further preferably 0.5% by mass or less. . Thereby, the effect by this invention as mentioned above is exhibited more reliably.
  • the coating layer covers at least a part of the mother particles. And the coating layer is comprised with the material containing at least 1 sort (s) selected from the group which consists of Au, Ag, Pt, Ni, and Pd.
  • the above metal elements may be included in the coating layer as a single metal or may be included as a constituent component of the alloy.
  • the coating layer only needs to be made of a material containing at least one selected from the group consisting of Au, Ag, Pt, Ni, and Pd. Among them, as the constituent material of the coating layer, at least Au and Ag are used. One is preferred.
  • Au and Ag are composite particles having a relatively low melting point among the metals constituting the group, even when sintered at a relatively low temperature in the production of a molded body as a sintered body. They can be suitably joined together. Moreover, the frequency characteristic of the magnetic permeability of the composite particles can be more suitably controlled by controlling the thickness of the coating layer.
  • the sum of the content ratios of Au and Ag in the coating layer is preferably 80% by mass or more, and more preferably 90% by mass or more. Thereby, the effects as described above are more remarkably exhibited.
  • the thickness of the coating layer is not particularly limited, but is preferably 10 nm or more and 500 nm or less, more preferably 20 nm or more and 400 nm or less, and further preferably 30 nm or more and 300 nm or less.
  • the thickness of the coating layer is determined by the following method. That is, after embedding the particles in a resin, the cross-sectional processing of the particles was performed using an ion milling device, and the obtained sample for photographing was produced. The obtained sample for photographing is photographed with FE-SEM, and the length of the scale included in the image analysis software or the image (value described), and the actual measurement value of the scale in the SEM image and the coating layer Calculated using the actual measured value with a thickness ruler. As the FE-SEM, SU-8020 manufactured by Hitachi High-Technologies was used. IM-4000 manufactured by Hitachi High-Technologies was used as the ion milling device. Epoxy resin was used as the embedding resin.
  • the average thickness (average length in the minor axis direction) of the composite particles is T0 [ ⁇ m] and the thickness of the coating layer is T1 [ ⁇ m]
  • the relationship of 0.0010 ⁇ T1 / T0 ⁇ 0.10 is satisfied. It is more preferable that the relationship of 0.0030 ⁇ T1 / T0 ⁇ 0.080 is satisfied, and it is more preferable that the relationship of 0.0050 ⁇ T1 / T0 ⁇ 0.050 is satisfied.
  • the average thickness (average length in the minor axis direction) is measured as described above.
  • the balance between electromagnetic wave absorption and electromagnetic wave reflection can be made more suitable, and the overall electromagnetic wave shielding effect can be made particularly excellent.
  • the composite particles of the present invention may have any structure as long as they include the mother particles and the coating layer as described above.
  • the composite particle may have at least one intermediate layer between the mother particle and the coating layer.
  • a coating layer made of a material other than Au, Ag, Pt, Ni, and Pd may be provided on the surface of the coating layer described above.
  • examples of such a coating layer include a surface treatment layer using various coupling agents such as a silane coupling agent.
  • first coating layer made of a material containing at least one selected from the group consisting of Au, Ag, Pt, Ni and Pd on the surface of the mother particle, Au
  • second coating layer made of a material other than Ag, Pt, Ni, and Pd may be provided.
  • the thickness of the coating layer is sufficiently smaller than the size of the mother particles, and the composite particles having the mother particles and the coating layer have substantially the same shape and size as the mother particles. Therefore, it is preferable that the composite particles have a plate shape and satisfy the same conditions as the size and shape of the mother particles described above. Thereby, the effects as described above are more reliably exhibited.
  • the composite particles preferably have a plate shape as a whole.
  • the average plate diameter (average length in the major axis direction) of the composite particles is preferably 10 ⁇ m or more and 2000 ⁇ m or less, more preferably 15 ⁇ m or more and 1000 ⁇ m or less, and further preferably 20 ⁇ m or more and 500 ⁇ m or less.
  • the average thickness (average length in the minor axis direction) of the composite particles is preferably 0.5 ⁇ m or more and 100 ⁇ m or less, more preferably 1.0 ⁇ m or more and 50 ⁇ m or less, and 2.0 ⁇ m or more and 30 ⁇ m or less. More preferably.
  • the aspect ratio of the composite particles is preferably 4 or more and 1000 or less, more preferably 4 or more and 300 or less, and even more preferably 4 or more and 200 or less.
  • the shape factor SF-2 of the composite particles is preferably 135 or more and 300 or less, more preferably 138 or more and 290 or less, and further preferably 140 or more and 280 or less.
  • the average value of the above conditions (average plate diameter, average thickness, aspect ratio, shape factor SF-2) for the plurality of composite particles is as follows: It is preferable that it is contained in the said range.
  • BET specific surface area of the powder (aggregate of composite particles) of the present invention is preferably equal to or less than 0.07 m 2 / g or more 3m 2 / g, 0.07m 2 / g or more 1.5 m 2 / g or less More preferably, it is 0.07 m 2 / g or more and 1 m 2 / g or less.
  • BET specific surface area of the mother particle of the present invention is preferably equal to or less than 0.05 m 2 / g or more 2.5 m 2 / g, more preferably not more than 0.05 m 2 / g or more 2m 2 / g, 0.05m and even more preferably 2 / g or more 0.85 m 2 / g or less.
  • the adhesiveness of the composite particles and the resin material in the molded body of the present invention can be further improved, and the durability of the molded body is particularly excellent. can do.
  • the BET specific surface area is determined by measurement using a specific surface area measuring device (model: Macsorb HM model-1208 (manufactured by Mountec)).
  • the tap density of the powder (aggregate of composite particles) of the present invention is preferably 1.0 g / cm 3 or more and 3.5 g / cm 3 or less, preferably 1.2 g / cm 3 or more and 2.5 g / cm 3 or less. It is more preferable that Thereby, it becomes easy to make high the filling rate of the composite particle in the molded object of this invention.
  • a tap density means the density calculated
  • a tapping device a USP tap density measuring device (Powder Tester PT-X, manufactured by Hosokawa Micron Corporation) or the like can be used.
  • the electric resistivity (volume resistivity) at 25 ° C. of the powder of the present invention is preferably 1 ⁇ 10 ⁇ 6 to 1 ⁇ 10 ⁇ 0 ⁇ ⁇ cm, and 1 ⁇ 10 ⁇ 6 to 1.0 ⁇ 10 ⁇ . It is more preferably 1 ⁇ ⁇ cm, and further preferably 1 ⁇ 10 ⁇ 6 to 1.0 ⁇ 10 ⁇ 2 ⁇ ⁇ cm.
  • the powder of the present invention only needs to contain a plurality of the composite particles of the present invention, and may further include particles other than the composite particles of the present invention.
  • the content of particles other than the composite particles of the present invention in the powder of the present invention is preferably 10% by mass or less, more preferably 5.0% by mass or less, and 1.0% More preferably, it is at most mass%.
  • the composite particles of the present invention can be produced by forming coating layers on the surface of plate-like ferrite particles produced by a predetermined method by various plating methods.
  • Examples of the plating method for forming the coating layer include wet plating methods such as electrolytic plating and electroless plating, and dry plating methods such as vacuum deposition, sputtering, and ion plating.
  • the wet plating method is preferable.
  • the electroless plating method is more preferable.
  • the ferrite particles to be the mother particles may be produced by any method, but can be suitably produced by, for example, the method described below.
  • the ferrite raw material is weighed and then mixed with a Henschel mixer or the like.
  • the ferrite raw material is not particularly limited, and examples thereof include metal oxides, metal carbonates, metal hydroxides, and mixtures thereof.
  • the obtained mixture of ferrite raw materials is pelletized with a roller compactor or the like, and pre-baked with a rotary kiln or the like to obtain a pre-fired product.
  • Pre-baking can be performed, for example, by heating in an air atmosphere.
  • the heating temperature at the time of pre-baking is not particularly limited, but is preferably 600 ° C or higher and 1200 ° C or lower, more preferably 650 ° C or higher and 1000 ° C or lower, and further preferably 700 ° C or higher and 900 ° C or lower. .
  • the obtained calcined product is roughly pulverized and finely pulverized to obtain a cake-like calcined product having an adjusted water content.
  • a dispersant is added to the cake-like temporarily fired product, the dispersion is dispersed using a dispersing device, and a binder is further added to prepare a liquid composition (a composition for producing a ferrite precursor).
  • the obtained liquid composition is applied on a substrate such as a film so as to have a predetermined thickness using an applicator or the like.
  • a sheet-like granulated product (ferrite precursor) containing a pre-fired product from the substrate after supplying the PVA aqueous solution to the surface to which the liquid composition has been applied and removing moisture. Peel off.
  • the binder removal treatment is preferably performed at the same or lower temperature than the main baking, and the treatment conditions are such that the binder component can be removed.
  • the heating temperature during the main baking is not particularly limited, but is preferably 600 ° C. or higher and 1400 ° C. or lower, more preferably 650 ° C. or higher and 1300 ° C. or lower, and further preferably 700 ° C. or higher and 1200 ° C. or lower.
  • the oxygen concentration in the atmosphere during the main firing is preferably 20% by volume or less, and more preferably 3.5% by volume or less.
  • the main baking can be suitably performed even in an air atmosphere.
  • the average plate diameter may be adjusted by subjecting the ferrite precursor before the main firing or the fired product after the main firing to a grinding treatment.
  • the pulverization treatment mother particles having a predetermined shape can be easily obtained.
  • the pulverization process can be suitably performed by, for example, pulverizing and classifying so as to obtain a target average plate diameter using a sieve having a predetermined aperture.
  • the adjustment of the average plate diameter by the pulverization treatment may be performed after the main calcination, but may be performed before the binder removal treatment and / or the main calcination in order to prevent adhesion between particles during the main calcination.
  • the plate-like ferrite particles that should be the mother particles have a crystal structure that is more easily distorted than bulk ferrite because the crystal growth direction is almost limited to the plane direction depending on the ferrite composition. Furthermore, when the grinding process is performed, the distortion of the crystal structure of the ferrite particles increases. Therefore, the distortion of the crystal structure can be reduced by performing a heat treatment after the pulverization process in addition to the main firing.
  • the heating temperature in the heat treatment is preferably 800 ° C. or higher and 1300 ° C. or lower.
  • the oxygen concentration in the atmosphere in the heat treatment is preferably 20% by volume or less, and more preferably 3.5% by volume or less.
  • the resin composition of the present invention contains the powder of the present invention described above and a resin material. Thereby, the resin composition which can be used suitably for manufacture of the molded object which is excellent in the shielding property of electromagnetic waves can be provided.
  • the resin material constituting the resin composition examples include epoxy resins, urethane resins, acrylic resins, silicone resins, various modified silicone resins (acrylic modified, urethane modified, epoxy modified, fluorine), polyamide resins, polyimide resins, and polyamideimides. Resins, fluorine and the like can be mentioned, and one or more selected from these can be used in combination.
  • the resin composition may contain components (other components) other than the powder and resin material of the present invention.
  • Such components include solvents, fillers (organic fillers, inorganic fillers), plasticizers, antioxidants, dispersants, colorants such as pigments, heat conductive particles (particles with high heat conductivity). ) And the like.
  • the ratio (content ratio) of the powder of the present invention to the total solid content in the resin composition is preferably 50% by mass to 95% by mass, and more preferably 80% by mass to 95% by mass.
  • a molded body produced using the resin composition while having excellent dispersion stability of the powder of the present invention in the resin composition, storage stability of the resin composition, moldability of the resin composition, and the like.
  • the mechanical strength, shielding properties of electromagnetic waves, and the like can be further improved.
  • the ratio (content ratio) of the resin material to the total solid content in the resin composition is preferably 5% by mass or more and 50% by mass or less, and more preferably 5% by mass or more and 20% by mass or less.
  • a molded body produced using the resin composition while having excellent dispersion stability of the powder of the present invention in the resin composition, storage stability of the resin composition, moldability of the resin composition, and the like.
  • the mechanical strength, shielding properties of electromagnetic waves, and the like can be further improved.
  • the molded body of the present invention is manufactured using a material containing the powder of the present invention and a resin material. Thereby, the molded object which is excellent in the shielding property of electromagnetic waves can be provided.
  • the shaped product of the present invention may be of any use, but is preferably an electromagnetic shielding material. Thereby, the effect by this invention as mentioned above is exhibited more notably.
  • the molded product of the present invention can be suitably produced using the resin composition of the present invention as described above.
  • the molding method of the molded body examples include compression molding, extrusion molding, injection molding, blow molding, calendar molding, various coating methods, and the like.
  • the molded body may be formed by, for example, directly applying a resin composition on a member on which the molded body is to be formed, or a target member (for example, a printed wiring) after being separately manufactured. It may be installed on a substrate or a metal foil (such as a copper foil).
  • the powder according to the present invention may be used without mixing and dispersing in a resin or the like without performing a process such as firing.
  • the powder is molded, granulated, or coated into a desired shape.
  • baking may be performed and used for manufacture of the molded object as a sintered compact.
  • the molded object of this invention should just contain the composite particle which concerns on this invention in the at least one part, for example, may have the area
  • pretreatment step intermediate step, post-treatment step
  • intermediate step post-treatment step
  • composite particles of the present invention are not limited to those manufactured by the method as described above, and may be manufactured by any method.
  • the composite particles, powder, and resin composition of the present invention have been representatively described for use in the production of an electromagnetic shielding material. You may use for manufacture other than an electromagnetic wave shielding material.
  • the composite particles and powder of the present invention may be used as magnetic core materials or fillers (particularly magnetic fillers).
  • the composite particles and powders of the present invention have a property that can be suitably detected by a metal detector. Therefore, the composite particle, powder, resin composition and molded product of the present invention may be used for the purpose of detection with a metal detector.
  • the composite particles and powder can be adjusted to a color tone other than black (for example, white to silver color tone).
  • the color tone of the molded product containing composite particles and powder is adjusted to a color tone other than black (for example, white to silver color tone) corresponding to the composite particles and powder, or a colorant is included in the molded product.
  • the molded product can be adjusted to a desired color tone. As a result, it can be suitably applied to various molded bodies applied to metal detectors.
  • the molded body of the present invention When the molded body of the present invention is applied to a metal detector, the molded body is provided on, for example, a base formed using a material other than the resin composition of the present invention and the surface of the base. And a surface layer formed using the resin composition of the present invention.
  • the molded body of the present invention When the molded body of the present invention is applied to a metal detector, the molded body preferably includes composite particles at least near the surface thereof. More specifically, the compact preferably contains composite particles in a region within 1.0 mm in the thickness direction from the surface, and the composite particles in a region within 0.5 mm in the thickness direction from the surface. It is more preferable that it contains.
  • the molded product of the present invention can be used for, for example, food production, processing, packaging (including packaging, the same applies hereinafter), cosmetics, and pharmaceuticals.
  • Foods are required to have high safety, but are generally manufactured, processed, and packaged in an environment where foreign substances are easily mixed. Therefore, by applying the present invention to an article used in the field of food production, processing, and packaging, a part of the article is separated, or at least a part of the article is mixed with another article. Etc. can be suitably detected.
  • the form of food in addition to solid form and semi-solid form (gel form of jelly, pudding, etc.), the form of food includes liquid, and the concept of food includes drinks and the like.
  • Food additives and supplements are also included in the concept of food.
  • natural products such as animal-derived meat, seafood, plant-derived vegetables, fruits, seeds, grains, beans, seaweed, and processed products thereof, artificial sweeteners, artificial seasonings such as artificial seasonings, etc.
  • New synthetic products are also included in the concept of food.
  • Examples of molded products used in the production and processing of food include cooking appliances, cooking utensils, cooking utensils, tableware, clothing (articles worn on the human body), and packaging members used for food packaging And articles used in association therewith, as well as articles used for maintenance and repair of these.
  • hot plate hot plate, stove, gas burner, oven, toaster, microwave oven, dishwasher, dish dryer, scale (scale), kitchen timer, thermometer, water purifier, water purification filter (cartridge) Cooking equipment such as pans, pans, kettles, lids, knives, scissors, ladle, spatula, peeler, slicer, mixer, chopper, masher, rolling pin, mudler, whisk, pestle, bowl, drainer Bowl, cutting board, mat, rice paddle, mold, die cutting, lye removal, grater (food grader), frying (turner), pick, drainer, sieve, mill, drop lid, ice tray, grill, tongs, egg slicer Cooking utensils such as bowls, measuring cups, measuring spoons; towels, kitchen paper, towels, towels, paper towels Cooking utensils such as draining sheets, wrap film, oven paper, squeezed bags, virtues, pans, etc .; dishes, cups, bowls, chopsticks (including chopsticks), spoons, for
  • Example 1 (1) Preparation of pre-baked product First, Fe 2 O 3 , Mn 3 O 4 and ZnO as raw materials were weighed at a predetermined ratio and mixed for 15 minutes with a Henschel mixer. After pelletizing the obtained mixture with a roller compactor, it was temporarily fired at a firing temperature of 950 ° C. in an air atmosphere using a rotary kiln to obtain a temporarily fired product.
  • a liquid composition was prepared from the obtained pre-baked product. First, the calcined product was coarsely pulverized with a rod mill, and then finely pulverized with a wet bead mill. Thereafter, a cake-like calcined product having a moisture content adjusted to 65% by mass was obtained. . A dispersant was added to the cake-like temporarily fired product, and the mixture was dispersed with a homogenizer. Further, 5% by mass of polyvinyl alcohol (PVA) with respect to the amount of water was added as a binder to prepare a liquid composition.
  • PVA polyvinyl alcohol
  • ferrite precursor was prepared using the obtained liquid composition. First, using a applicator, a liquid composition was applied onto a base material on a commercially available PET film (thickness 50 ⁇ m) so that the film thickness after drying (Dry thickness) was 10 ⁇ m. .
  • Pulverization treatment The obtained plate-like fired product was subjected to pulverization treatment (post-fired pulverization treatment) and classification treatment to obtain ferrite powder (aggregate of plate-like particles) serving as mother particles.
  • the obtained particles have an irregular shape and have an average thickness of 8.5 ⁇ m, an average plate diameter of 85.5 ⁇ m, an aspect ratio of 10.06, and an average value of the shape factor SF-2 of 215. there were.
  • the average surface roughness Ra was 0.85.
  • the BET specific surface area of the obtained ferrite powder was 0.11 m 2 / g.
  • the saturation magnetization was 86.2 emu / g
  • the residual magnetization was 3.7 emu / g
  • the coercive force was 26 Oe.
  • Comparative Example 1 A powder was produced in the same manner as in Example 1 except that the formation of the coating layer on the ferrite powder was omitted. That is, in this comparative example, the ferrite powder was used as a target powder as it was.
  • Comparative Example 2 A powder was produced in the same manner as in Example 1 except that spherical ferrite particles were used as the mother particles. That is, in this comparative example, the composite particles constituting the powder have spherical base particles and a coating layer made of Ag provided on the surface thereof, and the composite particles as a whole are spherical. It was a thing.
  • Comparative Example 3 A powder was produced in the same manner as in Comparative Example 2 except that the formation of the coating layer on the ferrite powder was omitted. That is, in this comparative example, spherical ferrite powder was used as a target powder as it was.
  • Tables 1 and 2 collectively show the configurations of the powders of the examples and comparative examples.
  • the color tone of the powder of the above example was white to silver, whereas the color tone of the powder of Comparative Example 1 was black.
  • the thickness of the coating layer was uniform in each part, and the composite particles as a whole had the same shape as the mother particles.
  • the content rate of components other than the ferrite in a mother particle was 0.1 mass% or less.
  • the content rate of components other than Ag in a coating layer was 0.1 mass% or less.
  • the content of Ag in the coating layer was determined by measurement using fluorescent X-rays. That is, in the above-mentioned Examples, the ferrite particles as the mother particles are mixed with Ag powder in a proportion of 5 parts by mass, 10 parts by mass, and 20 parts by mass, and further a fluororesin powder (Kynar 301F manufactured by Arkema Co.) as a binder resin.
  • the intensity of Ag was measured with a fluorescent X-ray measuring device (ZSX100s manufactured by Rigaku Corporation), and a calibration curve was prepared.
  • the intensity of Ag was measured with a fluorescent X-ray measuring apparatus, and the Ag content (ratio to 100% by mass of the mother particles (whole mother particles)) was calculated.
  • the content of components outside the composite particles in the powder was 0.1% by mass or less.
  • SF-2 was determined from the perimeter of each particle and the projected area based on the above formula, and the average value for 100 particles was defined as the shape factor SF-2.
  • FE-SEM was shot with SU-8020 manufactured by Hitachi High-Tech, with an acceleration voltage of 15 KV and a magnification of 200 times. Analysis was performed.
  • ⁇ Average thickness> 9 g of the powder to be measured and 1 g of the powder resin were put into a 50 cc glass bottle, mixed for 30 minutes with a ball mill, and the resulting mixture was put into a 13 mm diameter die and pressure-molded at a pressure of 30 MPa. Thereafter, the molded body was embedded in a resin in a vertically standing state so that a cross section of the molded body could be seen, and was polished with a polishing machine to obtain a sample for thickness measurement. Next, the prepared thickness measurement sample was photographed with an SEM having a magnification of 50 to 800 times, and the thickness (length in the minor axis direction) of the portion excluding the protrusions of the particles contained in the sample was measured. And the arithmetic average of the thickness of 100 particle
  • the BET specific surface area was determined by measurement using a specific surface area measuring device (model: Macsorb HM model-1208 (manufactured by Mountec)). More specifically, about 5 g of the measurement sample was put in a standard sample cell dedicated to a specific surface area measurement device, accurately weighed with a precision balance, and the measurement target powder (sample) was set in the measurement port, and measurement was started. The measurement was performed by a one-point method, and the BET specific surface area was automatically calculated when the weight of the sample was input at the end of the measurement.
  • a specific surface area measuring device model: Macsorb HM model-1208 (manufactured by Mountec)
  • VSM-C7-10A vibration sample type magnetometer
  • ⁇ ICP analysis> 0.2 g of ferrite powder to be measured is weighed, 60 ml of pure water plus 20 ml of 1N hydrochloric acid and 20 ml of 1N nitric acid is heated to prepare an aqueous solution in which the ferrite powder is completely dissolved, and an ICP analyzer (Shimadzu) The contents of Fe, Mn, Mg and Sr were measured using ICPS-1000IV manufactured by Seisakusho.
  • ⁇ Tap density> The tap density was measured using a tap density measuring device in accordance with JIS R1628.
  • the average surface roughness (Ra) was determined as follows. The surface roughness was measured according to JIS B 0601-2001. Measurement was performed on 100 particles randomly selected using a 3D laser microscope LEXT OLS4000 manufactured by Olympus, the surface roughness was calculated from the unevenness of the obtained surface particles, and the average value of the surface roughness of each particle obtained was calculated. Used as the average surface roughness Ra.
  • the Curie temperature and the thickness T of the coating layer in Table 1 were measured by the above methods.
  • FIG. 1 shows a cross-sectional SEM image of the composite particles of Example 1
  • FIG. 2 shows a cross-sectional EDX mapping image (Ag) of the composite particles of Example 1.
  • the obtained mixed liquid was poured into a mold for molding, and water was evaporated to produce a sheet-like molded body having a thickness of 1 mm.
  • the obtained sheet-like molded body was measured for electromagnetic wave shielding ability (attenuation rate) of magnetic field by the KEC method.
  • the electromagnetic wave shielding ability (attenuation rate) of the magnetic field was measured in the range of 0.1 MHz to 1 GHz.
  • FIG. 3 shows a representative example of the evaluation result. The evaluation results are determined according to the following criteria and are shown in Table 3.
  • B Relatively high damping force and sufficiently high shielding ability
  • C Although there is damping power but insufficient shielding ability
  • D Low damping ability and insufficient shielding ability
  • Electrodes were attached to both ends, and a weight of 1 kg was placed on top of the electrode, and the electrical resistance was measured. did.
  • the electrical resistance was measured by applying a measurement voltage of 1 V with a 2182A nanovolt meter manufactured by Keithley Co., Ltd., measuring the resistance after 60 seconds, and calculating the volume resistance.
  • the electromagnetic wave is preferably shielded by the metal coating (coating layer) present on the surface of the plate-like ferrite particles (mother particles) oriented in the molded body.
  • the metal coating coating layer
  • Comparative Examples 1 and 3 satisfactory results were not obtained because there was no metal coating.
  • Comparative Example 2 the spherical ferrite particles were subjected to silver coating (electroless plating), but sufficient radio wave shielding ability could not be obtained as compared with Example 3 having the same amount of silver coating. became.
  • the present invention can provide composite particles and powder excellent in electromagnetic wave shielding properties, can provide a molded body excellent in electromagnetic wave shielding properties, and can be suitably used for producing the molded body.
  • a resin composition can be provided.

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JP2006286729A (ja) * 2005-03-31 2006-10-19 Kobe Steel Ltd 電磁波吸収性および導電性に優れた塗料組成物、並びに該塗料組成物で被覆されている塗装金属板
KR20070097626A (ko) * 2006-03-28 2007-10-05 신경자 전자파 차폐 및 흡수용 프라이머 도료 및 그 제조방법
WO2016121619A1 (ja) * 2015-01-27 2016-08-04 パウダーテック株式会社 金属光沢を有する顔料用板状フェライト粒子

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JPH01223703A (ja) * 1988-03-02 1989-09-06 Hitachi Maxell Ltd 強磁性粉末とこれを用いた磁気記録媒体

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Publication number Priority date Publication date Assignee Title
JP2006286729A (ja) * 2005-03-31 2006-10-19 Kobe Steel Ltd 電磁波吸収性および導電性に優れた塗料組成物、並びに該塗料組成物で被覆されている塗装金属板
KR20070097626A (ko) * 2006-03-28 2007-10-05 신경자 전자파 차폐 및 흡수용 프라이머 도료 및 그 제조방법
WO2016121619A1 (ja) * 2015-01-27 2016-08-04 パウダーテック株式会社 金属光沢を有する顔料用板状フェライト粒子

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