WO2022186209A1 - 磁歪特性を有する組成物及びその硬化物 - Google Patents
磁歪特性を有する組成物及びその硬化物 Download PDFInfo
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- WO2022186209A1 WO2022186209A1 PCT/JP2022/008636 JP2022008636W WO2022186209A1 WO 2022186209 A1 WO2022186209 A1 WO 2022186209A1 JP 2022008636 W JP2022008636 W JP 2022008636W WO 2022186209 A1 WO2022186209 A1 WO 2022186209A1
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- component
- magnetostrictive
- composition
- meth
- acrylate
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- 239000000203 mixture Substances 0.000 title claims abstract description 81
- 239000000463 material Substances 0.000 claims abstract description 44
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- 239000007870 radical polymerization initiator Substances 0.000 claims abstract description 15
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 38
- 239000002245 particle Substances 0.000 claims description 34
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- XBYTTXAEDHUVAH-UHFFFAOYSA-N 2-(4-butoxyphenyl)-4,6-bis(trichloromethyl)-1,3,5-triazine Chemical compound C1=CC(OCCCC)=CC=C1C1=NC(C(Cl)(Cl)Cl)=NC(C(Cl)(Cl)Cl)=N1 XBYTTXAEDHUVAH-UHFFFAOYSA-N 0.000 description 1
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
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- 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
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
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- H10N35/80—Constructional details
- H10N35/85—Magnetostrictive active materials
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Definitions
- the present invention relates to a composition having magnetostrictive properties and a cured product thereof.
- a magnetostrictive material is a material that slightly deforms when a magnetic field is applied, and the phenomenon of this deformation is called “magnetostriction". Conversely, when force is applied to a magnetostrictive material to deform it, an inverse magnetostriction phenomenon occurs in which the magnetic field inside the material changes. A change in the magnetic field due to this inverse magnetostriction phenomenon can be used for sensors and vibration power generation. Magnetostriction is a property of ferromagnetic materials. Ferromagnetic materials such as Fe (iron), Co (cobalt), and Ni (nickel) can change at a rate of about 0.01 to 0.0001% with respect to the original shape.
- magnetostrictive materials having high magnetostrictive properties include Terfenol-D (Fe-Dy (dysprosium)-Tb (terbium) alloy), Galfenol (Fe-Ga (gallium) alloy), Fe-Co alloy It has been known.
- a magnetostrictive material As a magnetostrictive material, there has conventionally been proposed a composite reinforced magnetostrictive composite material in which a wire made of an iron-based magnetostrictive alloy is embedded as a filler in a base material (matrix). Specifically, the FeCo fiber reinforced composite material is obtained by arranging FeCo fibers as a filler in one direction in a mold and then pouring an epoxy resin base material into the mold and curing the resin under the condition that a predetermined stress is applied. is disclosed (see Patent Document 1).
- magnetostrictive materials whose surrounding magnetic field is changed by stress loading are expected to be used as energy harvesters or stress sensors by repeated stress loading.
- magnetostrictive materials such as Terfenol-D and Galfenol, which have high magnetostrictive properties, are brittle and therefore have the problem of being difficult to withstand repeated stress loads.
- the Fe—Co alloy which has slightly inferior magnetostrictive properties, has somewhat excellent mechanical properties, but still has insufficient fatigue properties.
- the present inventors adopted a powdery magnetostrictive material and newly developed a magnetostrictive composite material in which the magnetostrictive material is dispersed in a base material that hardens by radical polymerization. That is, in order to solve the above problems, the present invention employs the following configurations.
- a composition having magnetostrictive properties containing component (P): a compound containing a polymerizable group, component (M): a powdery magnetostrictive material, and component (R): a radical polymerization initiator.
- composition according to [2] The composition according to [1], wherein the component (M) is a group of particles made of an iron-based magnetostrictive alloy and having an average particle size of 5 ⁇ m or more and 50 ⁇ m or less.
- the content of the (M) component is 40% by volume or more and 60% by volume or less with respect to the total volume of the (P) component, the (M) component, and the (R) component,
- thermosetting elastomer is urethane (meth)acrylate.
- thermosetting elastomer has a weight average molecular weight obtained by reacting a polycaprolactone polyol having a number average molecular weight of 300 or more and 900 or less, an aliphatic or alicyclic diisocyanate, and a hydroxyl group-containing (meth)acrylate. is a urethane (meth)acrylate of 2000 or more and 30000 or less, the composition according to [7].
- a novel magnetostrictive composite material having magnetostrictive properties can be provided.
- FIG. 4 is a schematic view of component (M) particles dispersed in a cured product sample before and after application of a magnetic field when viewed from above.
- the arrow (z-axis direction) indicates the application direction of the magnetic field.
- FIG. 2(A) shows the state of the (M) component particles dispersed in the cured product sample before the application of the magnetic field.
- FIG. 2(B) shows the state (positive magnetostriction) of the (M) component particles dispersed in the cured product sample after the magnetic field was applied.
- FIG. 1 shows the state of the (M) component particles dispersed in the cured product sample before the application of the magnetic field.
- FIG. 2(B) shows the state (positive magnetostriction) of the (M) component particles dispersed in the cured product sample after the magnetic field was applied.
- FIG. 10 is a diagram showing a shape change of component (M) particles dispersed in a cured product sample, which is obtained by curing the composition of Example 6, upon application of a magnetic field.
- the vertical axis indicates magnetostriction, ⁇ (ppm).
- the horizontal axis indicates the magnetic flux density, ⁇ (mT).
- FIG. 10 is a diagram showing a shape change of component (M) particles dispersed in a cured product sample, which is obtained by curing the composition of Example 3, upon application of a magnetic field.
- the vertical axis indicates magnetostriction, ⁇ (ppm).
- the horizontal axis indicates the magnetic flux density, ⁇ (mT).
- composition having magnetostrictive properties contains (P) component: a compound containing a polymerizable group, (M) component: a powdery magnetostrictive material, and (R) component: a radical polymerization initiator, and magnetostrictive properties
- P component: a compound containing a polymerizable group
- M component: a powdery magnetostrictive material
- R component: a radical polymerization initiator
- the magnetostrictive property of this magnetostrictive composite material means at least the property of changing dimensions when a magnetic field is applied; and the property of changing the magnetic field inside the material when pressure is applied.
- the former property when a magnetic field is applied in one direction, the phenomenon of elongation in the same direction is called “positive magnetostriction”, and the phenomenon of contraction in the same direction is called “negative magnetostriction”.
- the compositions of the present invention can exhibit not only positive magnetostriction, but also negative magnetostriction.
- the form of the composition of the present embodiment is not particularly limited, and a preferred form is a form in which a powdery magnetostrictive material is dispersed in the composition.
- the form of the composition of the present embodiment may be, for example, a dispersion or solution, or may be powder or lump.
- the (P) component can be polymerized by the action of the (R) component when the composition is cured, and can constitute the base material (matrix) of the cured product.
- the “polymerizable group” in the component (P) is a group that enables a compound containing a polymerizable group to polymerize by radical polymerization or the like, and is a group that allows multiple A group containing a bond.
- the "polymerizable group" in the component (P) is not particularly limited, but is preferably radically polymerizable.
- the multiple bond between carbon atoms may be a polymerizable carbon-carbon double bond or a polymerizable carbon-carbon triple bond, preferably a polymerizable carbon-carbon double bond.
- Polymerizable carbon-carbon double bonds include, for example, methacryloyl groups and acryloyl groups.
- the number of polymerizable groups contained in the component (P) may be one, or two or more.
- the (P) component is preferably a thermosetting resin, more preferably a thermosetting resin containing a polymerizable unsaturated double bond, from the viewpoint of applications that take advantage of magnetostrictive properties.
- the number of polymerizable groups contained in the component (P) can be appropriately determined depending on the application.
- the (P) component includes a compound containing 1 to 6 polymerizable groups, and from the viewpoint of durability against repeated stress load and low elastic modulus, a compound containing 1 to 5 polymerizable groups is used. More preferred are compounds containing 1 to 4 polymerizable groups, and particularly preferred are compounds containing 1 or 2 polymerizable groups.
- the component (P) is preferably a thermosetting resin with a low glass transition temperature from the viewpoint of durability against repeated stress loads and a low elastic modulus, and a thermosetting resin with a glass transition temperature of 0 ° C. or less. is more preferred.
- glass transition temperature indicates a value measured by a test method conforming to JIS K 7244-1:1998 (ISO 6721-1:1994).
- the (P) component is preferably a thermosetting elastomer from the viewpoint of durability against repeated stress loads and low elastic modulus.
- a thermosetting elastomer tends to have a low elastic modulus after curing.
- Component (P) is more preferably a thermosetting elastomer with a glass transition temperature of 0°C or lower, more preferably a thermosetting elastomer with a glass transition temperature of -130°C or higher and -5°C or lower, Thermosetting elastomers having a glass transition temperature of -100°C to -5°C are particularly preferred, and thermosetting elastomers having a glass transition temperature of -50°C to -10°C are most preferred. If the glass transition temperature of the thermosetting elastomer as the component (P) is equal to or lower than the upper limit of the preferred range, the cured product can easily have a low elastic modulus. When it is at least the lower limit, the strength of the cured product can be enhanced.
- thermosetting elastomers include resin-based elastomers, and urethane (meth)acrylates are preferred.
- This urethane (meth)acrylate can be synthesized by an addition reaction of a polyol ((O) component), a polyisocyanate compound ((I) component), and a hydroxyl group-containing (meth)acrylate.
- a polyol ((O) component) a polyocyanate compound ((I) component)
- hydroxyl group-containing (meth)acrylate For example, it can be synthesized by performing a known urethanization reaction.
- (meth)acrylate is a concept including methacrylate and acrylate, and means methacrylate or acrylate.
- a polyol ((O) component) is a compound having two or more hydroxy groups (--OH).
- the (O) component is not particularly limited, and those commonly used in the production of urethane resins can be used without particular limitation.
- the (O) component may be either an aliphatic polyol or an aromatic polyol.
- the (O) component may be a low-molecular-weight polyol or a high-molecular-weight polyol.
- aliphatic is a concept relative to aromatics, meaning groups having no aromaticity, compounds having no aromaticity, etc. Define.
- alicyclic refers to a non-aromatic group or non-aromatic compound having a cyclic structure.
- low-molecular-weight polyols include ethylene glycol, 1,2-propylene glycol, 1,2-butanediol, 1,3-propylene glycol, 1,3-butanediol, 1,4-butanediol, 1,5 - pentanediol, 1,6-hexanediol, neopentyl glycol, alkanediol having 7 to 22 carbon atoms, diethylene glycol, triethylene glycol, dipropylene glycol, 3-methyl-1,5-pentanediol, 2-ethyl-2 -Butyl-1,3-propanediol, C17-20 alkane-1,2-diol, 1,3-cyclohexanedimethanol, 1,4-cyclohexanedimethanol, 1,4-cyclohexanediol, hydrogenated bisphenol A, dihydric alcohols such as 1,4-dihydroxy-2-butene, 2,6
- polymer polyols include phenolic resins, resins containing a hydroxystyrene skeleton, polyester polyols, polyether polyols, polyether ester polyols, polyesteramide polyols, acrylic polyols, polycarbonate polyols, polyhydroxyalkanes, polyurethane polyols, and polycaprolactones.
- polyols and vegetable oil-based polyols are preferred. These may be used alone, or two or more of them may be used in combination.
- the number average molecular weight of the polymer polyol is preferably 300-2000, more preferably 300-1500, even more preferably 300-900.
- Aliphatic diisocyanates, alicyclic diisocyanates, aromatic diisocyanates, or mixtures thereof can be used as polyisocyanate compounds (component (I)).
- Hexamethylene diisocyanate is preferred as the aliphatic diisocyanate.
- Preferred examples of the alicyclic diisocyanate include hydrogenated xylene diisocyanate, isophorone diisocyanate, 1,3-bisisocyanatomethylcyclohexane, 1,4-bisisocyanatomethylcyclohexane, norbornane diisocyanate, and dicyclohexylmethane-4,4'-diisocyanate. .
- aromatic diisocyanate 4,4-diphenylmethane diisocyanate is preferred.
- component (I) is preferably an aliphatic or alicyclic diisocyanate. These may be used alone, or two or more of them may be used in combination.
- a hydroxyl group-containing (meth)acrylate has at least one hydroxyl group and one or more (meth)acryloyl groups in one molecule.
- hydroxyl group-containing (meth)acrylates include unsaturated fatty acid hydroxyalkyl esters such as 2-hydroxyethyl (meth)acrylate, 2-hydroxypropyl (meth)acrylate, and 4-hydroxybutyl (meth)acrylate; ⁇ -caprolactone adduct of fatty acid hydroxyalkyl ester (average addition mole number 1-10); polyethylene glycol (average addition mole number 1-10) mono (meth) acrylate, polypropylene glycol (average addition mole number 1-10) mono ( meth)acrylate; pentaerythritol mono(meth)acrylate, pentaerythritol di(meth)acrylate, pentaerythritol tri(meth)acrylate; dipentaerythritol di(meth)acrylate, dipentaeryth
- the weight average molecular weight (Mw) of the thermosetting elastomer is preferably 2000 or more and 30000 or less, more preferably 2000 or more and 20000 or less, and even more preferably 3000 or more and 10000 or less.
- Mw of the thermosetting elastomer is at least the lower limit of the preferred range, the strength of the cured product tends to be increased. When this is done, it becomes easier to achieve a low elastic modulus.
- the weight average molecular weight (Mw) of a thermosetting elastomer means a value converted to standard polystyrene obtained by GPC measurement.
- the thermosetting elastomer has a weight average molecular weight obtained by reacting a polycaprolactone polyol having a number average molecular weight of 300 or more and 900 or less, an aliphatic or alicyclic diisocyanate, and a hydroxyl group-containing (meth)acrylate. is preferably urethane (meth)acrylate having a value of 2,000 or more and 30,000 or less.
- polyfunctional (meth)acrylate compound ⁇ Polyfunctional (meth)acrylate compound>> Moreover, you may use a polyfunctional (meth)acrylate compound as a (P) component.
- polyfunctional means having two or more functional groups.
- Multifunctional monomers include, for example, monomers with two functional groups, monomers with three functional groups, monomers with four functional groups, or monomers with more functional groups.
- Multifunctional acrylates include diacrylates, triacrylates, tetraacrylates.
- Polyfunctional methacrylates include dimethacrylate, trimethacrylate, and tetramethacrylate.
- polyfunctional (meth)acrylate compounds include ethoxylated (3) trimethylolpropane triacrylate, ethoxylated (3) trimethylolpropane trimethacrylate, ethoxylated (6) trimethylolpropane triacrylate, ethoxylated (9) trimethylolpropane triacrylate, ethoxylated (15) trimethylolpropane triacrylate, ethoxylated (20) trimethylolpropane triacrylate, pentaerythritol triacrylate, pentaerythritol trimethacrylate, propoxylated (3) glyceryl triacrylate, propoxylated ( 3) Glyceryl Triacrylate, Propoxylated (5.5) Glyceryl Triacrylate, Propoxylated (3) Trimethylolpropane Triacrylate, Propoxylated (6) Trimethylolpropane Triacrylate, Trimethylolpropane Triacrylate, Trimethylolpropane Trimethacrylate
- the (P) component may be used alone or in combination of two or more.
- the component (M) is a powdery material that slightly deforms when a magnetic field is applied.
- the average particle diameter of the particle group of component (M) is preferably 5 ⁇ m or more and 50 ⁇ m or less, more preferably 5 ⁇ m or more and 40 ⁇ m or less, and even more preferably 5 ⁇ m or more and 30 ⁇ m or less.
- the average particle size of the particle group of component (M) is at least the lower limit of the preferred range, good dispersibility is likely to be obtained. smoothness of the surface can be easily obtained.
- the average particle size of the particle group of component (M) was measured by a test method based on the particle size analysis-laser diffraction/scattering method specified in JIS Z 8825:2013. , indicates the volume average particle size.
- the (M) component consists of Ni, Fe—Ni alloy, Fe—Co alloy, Fe—Al alloy, Fe—Ga—Al alloy, Fe—Dy—Tb alloy, or Fe—Ga alloy.
- a metal particle group is mentioned.
- the (M) component is preferably composed of an iron-based magnetostrictive alloy.
- Fe—Co alloy, Fe—Ga—Al alloy, Fe—Dy—Tb alloy, and Fe—Ga alloy are preferably used, and Fe—Co alloy is more preferable. preferable.
- the specific example of the Fe--Ga--Al alloy is an FeGaAl alloy containing C (carbon) or B (boron).
- Fe--Dy--Tb alloys include, for example, Terfenol-D.
- Fe—Ga alloys include, for example, Galfenol.
- the (M) component may be used singly or in combination of two or more.
- the (M) component is preferably a group of particles made of an iron-based magnetostrictive alloy with an average particle size of 5 ⁇ m or more and 50 ⁇ m or less from the viewpoint of magnetostrictive properties and dispersion stability in the base material.
- the (R) component is a radical polymerization initiator, and when the composition is cured, it acts on the polymerizable groups of the (P) component to promote the polymerization reaction, contributing to the formation of the base material (matrix) of the cured product. do.
- the (R) component includes thermal radical polymerization initiators, photoradical polymerization initiators, and the like.
- Thermal radical polymerization initiators include, for example, peroxides and azo polymerization initiators.
- peroxides in the thermal radical polymerization initiator include ketone peroxides, peroxyketals, hydroperoxides, dialkyl peroxides and peroxyesters.
- specific examples of such peroxides include acetyl peroxide, dicumyl peroxide, tert-butyl peroxide, t-butyl cumyl peroxide, propionyl peroxide, benzoyl peroxide (BPO), 2-chlorobenzoyl peroxide, 3-chlorobenzoyl peroxide, 4-chlorobenzoyl peroxide, 2,4-dichlorobenzoyl peroxide, 4-bromomethylbenzoyl peroxide, lauroyl peroxide, potassium persulfate, diisopropyl peroxycarbonate, tetralin hydroperoxide, 1-phenyl -2-methylpropyl-1-hydroperoxide, tert-butyl pertriphenylacetate, tert-
- Examples of the above-mentioned peroxides include, for example, the trade name "Percumyl (registered trademark)", the trade name “Perbutyl (registered trade mark)", the trade name “Perloyl (registered trade mark)”, the trade name “Perocta (registered trademark)” and the like can be used.
- Examples of the azo polymerization initiator in the thermal radical polymerization initiator include 2,2′-azobispropane, 2,2′-dichloro-2,2′-azobispropane, 1,1′-azo(methylethyl ) diacetate, 2,2′-azobis(2-amidinopropane) hydrochloride, 2,2′-azobis(2-aminopropane) nitrate, 2,2′-azobisisobutane, 2,2′-azobisisobutyl Amide, 2,2'-azobisisobutyronitrile, methyl 2,2'-azobis-2-methylpropionate, 2,2'-dichloro-2,2'-azobisbutane, 2,2'-azobis-2 -methylbutyronitrile, 2,2'-azobis(2-methylpropionate) dimethyl(2,2'-azobisisobutyrate dimethyl), 1,1'-azobis(1-methylbutyronitrile-3-sodium sulfonate)
- Photoradical polymerization initiators include, for example, 1-hydroxycyclohexylphenyl ketone, 2-hydroxy-2-methyl-1-phenylpropan-1-one, 1-[4-(2-hydroxyethoxy)phenyl]-2- Hydroxy-2-methyl-1-propan-1-one, 1-(4-isopropylphenyl)-2-hydroxy-2-methylpropan-1-one, 1-(4-dodecylphenyl)-2-hydroxy-2 -methylpropan-1-one, 2,2-dimethoxy-1,2-diphenylethan-1-one, bis(4-dimethylaminophenyl)ketone, 2-methyl-1-[4-(methylthio)phenyl]- 2-morpholinopropan-1-one, 2-benzyl-2-dimethylamino-1-(4-morpholinophenyl)-butan-1-one, ethanone 1-[9-ethyl-6-(2-methylbenzoyl )-9
- photoradical polymerization initiator examples include "IRGACURE OXE02”, “IRGACURE OXE01”, “IRGACURE 369", “IRGACURE 651”, and “IRGACURE 907” (all trade names, manufactured by BASF); (trade name, manufactured by ADEKA Co., Ltd.) and the like can be used.
- the (R) component may be used singly or in combination of two or more.
- a thermal radical polymerization initiator is preferable, and among these, an azo polymerization initiator is more preferable.
- the total content of the (P) component, the (M) component and the (R) component in the composition of the present embodiment is preferably 80% by volume or more, more preferably 90% by volume or more. It is preferably 95% by volume or more, more preferably 100% by volume, or 100% by volume, that is, a composition consisting of the (P) component, the (M) component and the (R) component. preferable.
- the content of the (M) component is 10% by volume or more and 80 It is preferably vol% or less, and more preferably 20 vol% or more and 70 vol% or less. If the content of component (M) is within the above preferred range, the composition can exhibit both positive magnetostriction and negative magnetostriction. Further, when the content of the component (M) is at least the lower limit of the preferred range, the magnetostrictive properties are more likely to be exhibited. is enhanced.
- the content of the (M) component is set to It is preferably 40% by volume or more and 60% by volume or less, more preferably 45% by volume or more and 55% by volume or less, relative to the total volume (100% by volume).
- the composition of the present embodiment by controlling the volume fraction of the powdered magnetostrictive material in the cured product to a specific ratio, although the details are not clear, the composition is magnetized by applying a magnetic field. It is thought that the magnetostrictive material particles are attracted to each other, so that they exhibit negative magnetostrictive characteristics.
- the content of component (R) is preferably 0.01 parts by mass or more and 20 parts by mass or less with respect to 100 parts by mass of component (P). It is more preferably 0.5 parts by mass or more and 10 parts by mass or less, more preferably 0.5 parts by mass or more and 10 parts by mass or less. If the content of the component (R) is at least the lower limit of the preferred range, the efficiency of the polymerization reaction between the components (P) is further improved. The reaction is sufficiently accelerated, and the strength of the cured product is further enhanced.
- composition of the present embodiment may contain other components other than these, if necessary.
- Other components other than the (P) component, the (M) component and the (R) component include, for example, solvents, surfactants, dispersants, antifoaming agents, antioxidants, fragrances, plasticizers and the like.
- composition of the present embodiment can be prepared by a production method comprising a step of mixing the (P) component, the (M) component, the (R) component, and optionally other components.
- the composition of the present embodiment includes a first step of mixing the (P) component and the (R) component to obtain a mixture (PR), and the mixture (PR) obtained in the first step and the (M) component It can also be prepared by a manufacturing method having a second step of mixing.
- the composition can exhibit both positive magnetostriction and negative magnetostriction.
- the cured product of the present embodiment is obtained by curing the above-described (composition having magnetostrictive properties).
- the shape of the cured product is not particularly limited, and examples thereof include a plate shape, a cylindrical shape, and a prismatic shape.
- the cured product of the present embodiment can be produced, for example, by a production method comprising the steps of pouring the above-described composition into a mold having a predetermined shape and performing heat curing treatment.
- the heat curing treatment may be performed in one operation, or may be performed in two or more operations.
- the composition of the present embodiment includes (P) component: a compound containing a polymerizable group, (M) component: a powdery magnetostrictive material, and (R) component: a radical polymerization initiator,
- P component: a compound containing a polymerizable group
- M component: a powdery magnetostrictive material
- R component: a radical polymerization initiator
- It is a magnetostrictive composite material containing and having magnetostrictive properties. That is, it is a novel magnetostrictive composite material in which a powdery magnetostrictive material is employed and the magnetostrictive material is dispersed in a base material that is hardened by radical polymerization. Therefore, unlike a conventional form in which a wire made of an iron-based magnetostrictive alloy is embedded in a base material (matrix) as a filler (filler), there is no complexity and simple handling is possible.
- the polymerizable compound that constitutes the base material can be selected, it is possible to provide a magnetostrictive composite material in which a magnetostrictive material and various polymers are combined.
- a magnetostrictive composite material for example, a magnetostrictive composite material that can withstand repeated stress loads can be provided by combining a magnetostrictive material and a low elastic modulus polymer.
- the composition of the present embodiment can also be applied to applications such as composite material substrates.
- fiber reinforced plastic such as glass fiber reinforced plastic or carbon fiber reinforced plastic and a sheet made of the composition of the present embodiment or a cured product thereof are laminated and cured to provide an FRP bulk having a magnetostrictive effect. can do.
- composition of the present embodiment by controlling the mixing ratio of the polymerizable compound constituting the base material and the powdery magnetostrictive material, not only positive magnetostriction (extending in the direction of magnetic field application) but also It is also possible to provide magnetostrictive composites that exhibit negative magnetostriction (shortening in the direction of applied magnetic field).
- composition of this embodiment compared with a single magnetostrictive material, it can be expected to further improve energy harvesting and stress sensor functions when bending stress or bending vibration is used.
- the composition of such an embodiment is useful as a smart material because it is a kind of material that causes some kind of reaction to an external stimulus.
- Component (P) Compound containing a polymerizable group
- Compound (P-1) Urethane acrylate (product name: DA-800AU, NOF Corporation) is used as a thermosetting elastomer resin. The glass transition temperature of the cured product is minus 30°C.
- Compound (P-1) is obtained by reacting polycaprolactone diol having a number average molecular weight of 530, isophorone diisocyanate, and 2-hydroxyethyl acrylate. The weight average molecular weight of compound (P-1) is 5,200.
- Compound (P-2) Dipentaerythritol hexaacrylate (trade name KAYARAD DPHA, Nippon Kayaku Co., Ltd.) is used as a thermosetting resin.
- the glass transition temperature of the cured product exceeds 250°C.
- Powdered magnetostrictive material Fe49Co49V2 Epson Atmix Corporation
- Average particle size 8.0 ⁇ 1.0 ⁇ m.
- Example 1 3 parts by mass of component (R) was added to 100 parts by mass of compound (P-1) and dissolved by stirring to obtain a uniform solution.
- the component (M) was added so as to have the volume fraction shown in Table 1, and the mixture was stirred to prepare a composition, which is a dispersion liquid in which the powdery magnetostrictive material is dispersed.
- the volume fraction was calculated assuming that the density of Fe 49 Co 49 V 2 (M) component was 8.6 g/cm 3 and the density of compound (P-1) and component (R) was 1.0 g/cm 3 . .
- Example 2-4 A composition, which is a dispersion liquid in which a powdery magnetostrictive material is dispersed, was prepared in the same manner as in Example 1, except that the volume fraction was changed as shown in Table 1.
- Example 5 3 parts by mass of component (R) was added to 100 parts by mass of compound (P-2) and dissolved by stirring to obtain a homogeneous solution.
- the component (M) was added so as to have the volume fraction shown in Table 2, and the mixture was stirred to prepare a composition, which is a dispersion liquid in which the powdery magnetostrictive material is dispersed.
- the volume fraction was calculated assuming that the density of Fe 49 Co 49 V 2 (M) component was 8.6 g/cm 3 and the density of compound (P-2) and (R) component was 1.0 g/cm 3 . .
- Examples 6-8) A composition, which is a dispersion liquid in which a powdery magnetostrictive material is dispersed, was prepared in the same manner as in Example 5, except that the volume fraction was changed as shown in Table 2.
- Each example composition was cast into a 10 mm ⁇ 10 mm ⁇ 2 mm mold. After that, each mold was placed on a ceramic hot plate (CHP-170DF (AS ONE)) and heat-cured at 80°C for 2 hours under nitrogen flow, followed by heating at 120°C for 1 hour. A cured product sample was obtained by performing a curing treatment.
- CHP-170DF AS ONE
- FIG. 1 is a schematic diagram showing a method for evaluating magnetostrictive characteristics in this example.
- a cured product sample 20 is placed between a pair of electromagnets 10,10.
- An orthogonal strain gauge 30 is attached to a 6 mm square area on the surface of the cured product sample 20, and the electromagnet 10 applies a magnetic field from minus 1 tesla to plus 1 tesla to the surface of the cured product sample 20 in a horizontal direction and at the same time. It was applied in the direction (z-axis direction).
- the direction horizontal to the surface of the cured product sample 20 and orthogonal to the z-axis direction is defined as the x-axis direction.
- the deformation state of the cured product sample 20 at that time was evaluated using a vibrating sample magnetometer. The evaluation results are shown in Tables 1-2 and FIGS. 2-4, respectively.
- FIG. 2 is a schematic plan view of component (M) particles dispersed in a cured product sample before and after application of a magnetic field.
- the arrow (z-axis direction) indicates the application direction of the magnetic field.
- FIG. 2(A) shows the state of the (M) component particles 20a dispersed in the cured product sample before the magnetic field is applied, and has a substantially circular shape in plan view.
- FIG. 2(B) shows the state of the (M) component particles dispersed in the cured product sample after the magnetic field was applied.
- the (M) component particles 22b are elongated in the magnetic field application direction after the magnetic field is applied, and the major axis is the z-axis in plan view. It has a substantially elliptical shape that is parallel to the . That is, a composition in which such (M) component particles are dispersed has positive magnetostriction.
- FIG. 2(C) shows the state of the (M) component particles dispersed in the cured product sample after the magnetic field was applied.
- the (M) component particles 24c are shortened in the magnetic field application direction after the magnetic field is applied, and in plan view, the major axis is the z-axis. It has a substantially elliptical shape perpendicular to the . That is, a composition in which such (M) component particles are dispersed has negative magnetostrictive properties.
- FIG. 3 is a diagram showing the shape change of the (M) component particles dispersed in the cured product sample with the application of a magnetic field for the cured product obtained by curing the composition of Example 6.
- the vertical axis indicates magnetostriction, ⁇ (ppm).
- the horizontal axis indicates the magnetic flux density, ⁇ (mT).
- Example 6 With respect to the composition of Example 6, the cured product sample expands in the z-axis direction, which is the direction of magnetic field application, and contracts in the x-axis direction, which is the direction perpendicular to the direction of magnetic field application, with the application of a magnetic field. was confirmed.
- FIG. 4 is a diagram showing the shape change of the (M) component particles dispersed in the cured product sample with the application of a magnetic field for the cured product obtained by curing the composition of Example 3.
- the vertical axis indicates magnetostriction, ⁇ (ppm).
- the horizontal axis indicates the magnetic flux density, ⁇ (mT).
- Example 3 With respect to the composition of Example 3, the cured product sample contracted in the z-axis direction, which is the direction in which the magnetic field was applied, with the application of the magnetic field, and slightly expanded and contracted in the x-axis direction, which is the direction perpendicular to the direction in which the magnetic field was applied. A negative magnetostrictive characteristic was confirmed.
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Abstract
Description
本願は、2021年3月1日に日本に出願された、特願2021-031516号に基づき優先権主張し、その内容をここに援用する。
逆に、磁歪材料に力を加えて変形させると、材料内部の磁場が変化する逆磁歪現象が起こる。この逆磁歪現象による磁場の変化を、センサや振動発電に利用することができる。 磁歪は、強磁性体の特性である。Fe(鉄)、Co(コバルト)、Ni(ニッケル)などの強磁性体では、元の形状に対して約0.01~0.0001%の割合で変化し得る。また、超磁歪と言われる、高い磁歪特性を有する磁歪材料として、Terfenol-D(Fe-Dy(ジスプロシウム)-Tb(テルビウム)合金)、Galfenol(Fe-Ga(ガリウム)合金)、Fe-Co合金が知られている。
具体的には、充填材としてFeCoファイバを、型の中で一方向に配列し、所定の応力を負荷した状態で、エポキシ樹脂母材を型に流し込んで硬化させてなる、FeCoファイバ強化複合材料が開示されている(特許文献1参照)。
しかしながら、Terfenol-D、Galfenol等の高い磁歪特性を有する磁歪材料には、それ自体が脆いために、繰り返し応力負荷に耐えられにくい問題がある。磁歪特性のやや劣るFe-Co合金は、力学特性にやや優れるものの、疲労特性は依然として不充分である。
本発明は、上記事情に鑑みてなされたものであり、磁歪特性を有する新規な磁歪複合材料を提供すること、を課題とする。
本実施形態の組成物は、(P)成分:重合性基を含む化合物と、(M)成分:粉末状の磁歪材料と、(R)成分:ラジカル重合開始剤と、を含有し、磁歪特性を有する磁歪複合材料である。
前者の性質において、磁場を一方向へ加えて、その同じ方向へ伸長する現象を「正の磁歪」といい、その同じ方向へ短縮する現象を「負の磁歪」という。
本実施形態の組成物は、正の磁歪を示すのみならず、負の磁歪も示し得るものである。
また、本実施形態の組成物の形態は、例えば、分散液もしくは溶液でもよいし、又は、粉末状もしくは塊状でもよい。
(P)成分は、組成物を硬化させた際、(R)成分の作用により重合して、硬化物の母材(マトリックス)を構成し得るものである。
(P)成分における「重合性基」とは、重合性基を含む化合物がラジカル重合等により重合することを可能とする基であり、例えば重合性不飽和二重結合などの炭素原子間の多重結合を含む基をいう。
炭素原子間の多重結合は、重合性炭素-炭素二重結合であってもよいし、重合性炭素-炭素三重結合であってもよいが、重合性炭素-炭素二重結合が好ましい。重合性炭素-炭素二重結合としては、例えば、メタクリロイル基、アクリロイル基が挙げられる。
(P)成分が含む重合性基は、1種であってもよく、2種以上であってもよい。
例えば、(P)成分としては、重合性基1~6個を含む化合物が挙げられ、繰り返し応力負荷に対する耐久性、低弾性率化などの観点から、重合性基1~5個を含む化合物が好ましく、重合性基1~4個を含む化合物がさらに好ましく、重合性基1又は2個を含む化合物が特に好ましい。
本明細書及び本特許請求の範囲において、「ガラス転移温度」は、JIS K 7244-1:1998(ISO 6721-1:1994)に準拠した試験方法により測定した値を示す。
(P)成分として熱硬化性エラストマーのガラス転移温度が、前記の好ましい範囲の上限値以下であれば、硬化物とした際、低弾性率化が図られやすくなり、一方、前記の好ましい範囲の下限値以上であると、硬化物とした際の強度が高められる。
熱硬化性エラストマーとしては、例えば樹脂系エラストマーが挙げられ、ウレタン(メタ)アクリレートが好適に挙げられる。
このウレタン(メタ)アクリレートは、ポリオール((O)成分)と、ポリイソシアネート化合物((I)成分)と、水酸基含有(メタ)アクリレートとの付加反応により合成することができる。例えば、公知のウレタン化反応を行うことにより合成できる。
ここで「(メタ)アクリレート」は、メタクリレート及びアクリレートを包含する概念であり、メタクリレート又はアクリレートを意味する。
(O)成分は、脂肪族ポリオールであってもよいし、芳香族ポリオールであってもよい。あるいは、(O)成分は、低分子ポリオールであってもよいし、高分子ポリオールであってもよい。
前記脂環式ジイソシアネートとしては、水添キシレンジイソシアネート、イソホロンジイソシアネート、1,3-ビスイソシアナトメチルシクロヘキサン、1,4-ビスイソシアナトメチルシクロヘキサン、ノルボルナンジイソシアネート、ジシクロヘキシルメタン-4,4’-ジイソシアネートが好ましい。
前記芳香族ジイソシアネートとしては、4,4-ジフェニルメタンジイソシアネートが好ましい。
これらの中でも、(I)成分は、脂肪族又は脂環式ジイソシアネートが好ましい。
これらは単独で用いてもよく、2種以上を併用して用いることもできる。
水酸基含有(メタ)アクリレートとしては、例えば、2-ヒドロキシエチル(メタ)アクリレート、2-ヒドロキシプロピル(メタ)アクリレート、4-ヒドロキシブチル(メタ)アクリレートなどの不飽和脂肪酸ヒドロキシアルキルエステル;前記の不飽和脂肪酸ヒドロキシアルキルエステルのε-カプロラクトン付加物(平均付加モル数1~10);ポリエチレングリコール(平均付加モル数1~10)モノ(メタ)アクリレート、ポリプロピレングリコール(平均付加モル数1~10)モノ(メタ)アクリレート;ペンタエリスリトールモノ(メタ)アクリレート、ペンタエリスリトールジ(メタ)アクリレート、ペンタエリスリトールトリ(メタ)アクリレート;ジペンタエリスリトールジ(メタ)アクリレート、ジペンタエリスリトールトリ(メタ)アクリレート、ジペンタエリスリトールテトラ(メタ)アクリレート、ジペンタエリスリトールペンタ(メタ)アクリレート;グリセリンモノ(メタ)アクリレート、ジグリセリントリ(メタ)アクリレート、ジグリセリンジ(メタ)アクリレート;ソルビトールモノ(メタ)アクリレート、ソルビトールジ(メタ)アクリレート、ソルビトールトリ(メタ)アクリレート、ソルビトールテトラ(メタ)アクリレート等が挙げられる。
これらの中でも、水酸基含有(メタ)アクリレートは、不飽和脂肪酸ヒドロキシアルキルエステルが好ましい。
これら水酸基含有(メタ)アクリレートは、1種単独で用いてもよく、2種以上を組み合わせてもよい。
熱硬化性エラストマーのMwが、前記の好ましい範囲の下限値以上であると、硬化物とした際の強度が高められやすくなり、一方、前記の好ましい範囲の上限値以下であると、硬化物とした際、低弾性率化が図られやすくなる。
本明細書及び本特許請求の範囲において、熱硬化性エラストマーの重量平均分子量(Mw)は、GPC測定により求めた標準ポリスチレン換算の値を意味する。
また、(P)成分としては、多官能(メタ)アクリレート化合物を用いてもよい。
本明細書において、「多官能性」とは、2つ以上の官能基を有することを意味する。多官能性モノマーは、例えば、2つの官能基を有するモノマー、3つの官能基を有するモノマー、4つの官能基を有するモノマーを包含し、又はさらに多くの官能基を有するモノマーを包含する。多官能アクリレートには、ジアクリレート、トリアクリレート、テトラアクリレートが含まれる。また、多官能メタクリレートには、ジメタクリレート、トリメタクリレート、テトラメタクリレートが含まれる。
(M)成分は、磁場を加えると僅かに変形する材料であって粉末状のものである。
(M)成分の粒子群の平均粒径は、5μm以上50μm以下であることが好ましく、5μm以上40μm以下がより好ましく、5μm以上30μm以下がさらに好ましい。
(M)成分の粒子群の平均粒径が、前記の好ましい範囲の下限値以上であると、良好な分散性が得られやすくなり、一方、前記の好ましい範囲の上限値以下であると、良好な表面の平滑性が得られやすくなる。
本明細書及び本特許請求の範囲において、(M)成分の粒子群の平均粒径は、JIS Z 8825:2013で規定される粒子径解析-レーザ回折・散乱法に準拠した試験方法により測定した、体積平均粒径を示す。
これらの中でも、(M)成分は、鉄基磁歪合金からなるものが好ましい。鉄基磁歪合金としては、Fe-Co系合金、Fe-Ga-Al系合金、Fe-Dy-Tb系合金、Fe-Ga系合金を用いることが好ましく、Fe-Co系合金を用いることがより好ましい。
Fe-Ga-Al系合金の前記具体例は、C(炭素)又はB(ホウ素)含むFeGaAl系の合金である。
Fe-Ga系合金には、例えばGalfenolが挙げられる。
(R)成分は、ラジカル重合開始剤であり、組成物を硬化させる際、(P)成分の重合性基に作用して重合反応を促進し、硬化物の母材(マトリックス)の形成に寄与する。 (R)成分としては、熱ラジカル重合開始剤、光ラジカル重合開始剤等が挙げられる。
熱ラジカル重合開始剤としては、例えば過酸化物、アゾ系重合開始剤が挙げられる。
このような過酸化物として具体的には、過酸化アセチル、過酸化ジクミル、過酸化tert-ブチル、過酸化t-ブチルクミル、過酸化プロピオニル、過酸化ベンゾイル(BPO)、過酸化2-クロロベンゾイル、過酸化3-クロロベンゾイル、過酸化4-クロロベンゾイル、過酸化2,4-ジクロロベンゾイル、過酸化4-ブロモメチルベンゾイル、過酸化ラウロイル、過硫酸カリウム、ペルオキシ炭酸ジイソプロピル、テトラリンヒドロペルオキシド、1-フェニル-2-メチルプロピル-1-ヒドロペルオキシド、過トリフェニル酢酸-tert-ブチル、tert-ブチルヒドロペルオキシド、過ギ酸tert-ブチル、過酢酸tert-ブチル、過安息香酸tert-ブチル、過フェニル酢酸tert-ブチル、過4-メトキシ酢酸tert-ブチル、過N-(3-トルイル)カルバミン酸tert-ブチル等が挙げられる。
光ラジカル重合開始剤としては、例えば、1-ヒドロキシシクロヘキシルフェニルケトン、2-ヒドロキシ-2-メチル-1-フェニルプロパン-1-オン、1-〔4-(2-ヒドロキシエトキシ)フェニル〕-2-ヒドロキシ-2-メチル-1-プロパン-1-オン、1-(4-イソプロピルフェニル)-2-ヒドロキシ-2-メチルプロパン-1-オン、1-(4-ドデシルフェニル)-2-ヒドロキシ-2-メチルプロパン-1-オン、2,2-ジメトキシ-1,2-ジフェニルエタン-1-オン、ビス(4-ジメチルアミノフェニル)ケトン、2-メチル-1-〔4-(メチルチオ)フェニル〕-2-モルフォリノプロパン-1-オン、2-ベンジル-2-ジメチルアミノ-1-(4-モルフォリノフェニル)-ブタン-1-オン、エタノン1-[9-エチル-6-(2-メチルベンゾイル)-9H-カルバゾール-3-イル]-1-(o-アセチルオキシム)、2,4,6-トリメチルベンゾイルジフェニルホスフィンオキシド、4-ベンゾイル-4’-メチルジメチルスルフィド、4-ジメチルアミノ安息香酸、4-ジメチルアミノ安息香酸メチル、4-ジメチルアミノ安息香酸エチル、4-ジメチルアミノ安息香酸ブチル、4-ジメチルアミノ-2-エチルヘキシル安息香酸、4-ジメチルアミノ-2-イソアミル安息香酸、ベンジル-β-メトキシエチルアセタール、ベンジルジメチルケタール、1-フェニル-1,2-プロパンジオン-2-(o-エトキシカルボニル)オキシム、o-ベンゾイル安息香酸メチル、2,4-ジエチルチオキサントン、2-クロロチオキサントン、2,4-ジメチルチオキサントン、1-クロロ-4-プロポキシチオキサントン、チオキサンテン、2-クロロチオキサンテン、2,4-ジエチルチオキサンテン、2-メチルチオキサンテン、2-イソプロピルチオキサンテン、2-エチルアントラキノン、オクタメチルアントラキノン、1,2-ベンズアントラキノン、2,3-ジフェニルアントラキノン、アゾビスイソブチロニトリル、ベンゾイルパーオキシド、クメンパーオキシド、2-メルカプトベンゾイミダール、2-メルカプトベンゾオキサゾール、2-メルカプトベンゾチアゾール、2-(o-クロロフェニル)-4,5-ジフェニルイミダゾール二量体、2-(o-クロロフェニル)-4,5-ジ(メトキシフェニル)イミダゾール二量体、2-(o-フルオロフェニル)-4,5-ジフェニルイミダゾール二量体、2-(o-メトキシフェニル)-4,5-ジフェニルイミダゾール二量体、2-(p-メトキシフェニル)-4,5-ジフェニルイミダゾール二量体、2,4,5-トリアリールイミダゾール二量体、ベンゾフェノン、2-クロロベンゾフェノン、4,4’-ビスジメチルアミノベンゾフェノン(すなわち、ミヒラーズケトン)、4,4’-ビスジエチルアミノベンゾフェノン(すなわち、エチルミヒラーズケトン)、4,4’-ジクロロベンゾフェノン、3,3-ジメチル-4-メトキシベンゾフェノン、ベンジル、ベンゾイン、ベンゾインメチルエーテル、ベンゾインエチルエーテル、ベンゾインイソプロピルエーテル、ベンゾイン-n-ブチルエーテル、ベンゾインイソブチルエーテル、ベンゾイン-t-ブチルエーテル、アセトフェノン、2,2-ジエトキシアセトフェノン、p-ジメチルアセトフェノン、p-ジメチルアミノプロピオフェノン、ジクロロアセトフェノン、トリクロロアセトフェノン、p-t-ブチルアセトフェノン、p-ジメチルアミノアセトフェノン、p-t-ブチルトリクロロアセトフェノン、p-t-ブチルジクロロアセトフェノン、α,α-ジクロロ-4-フェノキシアセトフェノン、チオキサントン、2-メチルチオキサントン、2-イソプロピルチオキサントン、ジベンゾスベロン、ペンチル-4-ジメチルアミノベンゾエート、9-フェニルアクリジン、1,7-ビス-(9-アクリジニル)ヘプタン、1,5-ビス-(9-アクリジニル)ペンタン、1,3-ビス-(9-アクリジニル)プロパン、p-メトキシトリアジン、2,4,6-トリス(トリクロロメチル)-s-トリアジン、2-メチル-4,6-ビス(トリクロロメチル)-s-トリアジン、2-[2-(5-メチルフラン-2-イル)エテニル]-4,6-ビス(トリクロロメチル)-s-トリアジン、2-[2-(フラン-2-イル)エテニル]-4,6-ビス(トリクロロメチル)-s-トリアジン、2-[2-(4-ジエチルアミノ-2-メチルフェニル)エテニル]-4,6-ビス(トリクロロメチル)-s-トリアジン、2-[2-(3,4-ジメトキシフェニル)エテニル]-4,6-ビス(トリクロロメチル)-s-トリアジン、2-(4-メトキシフェニル)-4,6-ビス(トリクロロメチル)-s-トリアジン、2-(4-エトキシスチリル)-4,6-ビス(トリクロロメチル)-s-トリアジン、2-(4-n-ブトキシフェニル)-4,6-ビス(トリクロロメチル)-s-トリアジン、2,4-ビス-トリクロロメチル-6-(3-ブロモ-4-メトキシ)フェニル-s-トリアジン、2,4-ビス-トリクロロメチル-6-(2-ブロモ-4-メトキシ)フェニル-s-トリアジン、2,4-ビス-トリクロロメチル-6-(3-ブロモ-4-メトキシ)スチリルフェニル-s-トリアジン、2,4-ビス-トリクロロメチル-6-(2-ブロモ-4-メトキシ)スチリルフェニル-s-トリアジン等が挙げられる。
(M)成分の含有量が前記の好ましい範囲内であれば、組成物は正の磁歪、負の磁歪をいずれも示し得る。
また、(M)成分の含有量が、前記の好ましい範囲の下限値以上であると、磁歪特性がより発現しやすくなり、一方、前記の好ましい範囲の上限値以下であると、硬化物の強度がより高められる。
このように、本実施形態の組成物においては、硬化物中に占める、粉末状の磁歪材料の体積分率を特定の割合に制御することで、詳細は定かではないが、磁場印加によって磁化した磁歪材料粒子同士が相互に引き合うため、負の磁歪特性を示すようになる、と考えられる。
(R)成分の含有量が、前記の好ましい範囲の下限値以上であれば、(P)成分間の重合反応効率がより向上し、一方、前記の好ましい範囲の上限値以下であれば、重合反応が充分に促進され、また、硬化物の強度がより高められる。
本実施形態の組成物は、(P)成分、(M)成分及び(R)成分に加え、これら以外のその他成分を必要に応じて含有してもよい。
(P)成分、(M)成分及び(R)成分以外のその他成分としては、例えば、溶剤、界面活性剤、分散剤、消泡剤、酸化防止剤、香料、可塑剤等が挙げられる。
本実施形態の組成物は、(P)成分と、(M)成分と、(R)成分と、必要に応じてその他成分と、を混合する工程を有する製造方法により調製することができる。
第2工程において、混合物(PR)と(M)成分との混合比率(体積比)は、(M)成分/混合物(PR)=10/90~80/20とすることが好ましく、20/80~70/30とすることがより好ましい。混合物(PR)と(M)成分との体積比を、前記の好ましい範囲内に制御することで、組成物は正の磁歪、負の磁歪をいずれも示し得るようになる。
さらに、組成物が負の磁歪を示し得るようになることから、第2工程において、混合物(PR)と(M)成分との混合比率(体積比)は、(M)成分/混合物(PR)=40/60~60/40とすることが好ましく、45/55~55/45とすることがより好ましい。
本実施形態の硬化物は、上述の(磁歪特性を有する組成物)が硬化したものである。 硬化物の形状は、特に限定されず、例えば板状、円柱状、角柱状が挙げられる。
本実施形態の硬化物は、例えば、上述の組成物を、所定形状の型に流し込み、熱硬化処理を行う工程を有する製造方法により製造することができる。
熱硬化処理は、1回の操作で行ってもよいし、2回以上の操作で行ってもよい。
かかる磁歪複合材料として、例えば、磁歪材料と、低弾性率ポリマーとの複合化によって、繰り返し応力負荷に耐えられる磁歪複合材料を提供することができる。
あるいは、本実施形態の組成物は、複合材料の基材のような用途にも適用することができる。例えば、ガラス繊維強化プラスチック又は炭素繊維強化プラスチック等の繊維強化プラスチックと、本実施形態の組成物もしくはその硬化物からなるシートと、を積層して硬化させることにより、磁歪効果を有するFRPバルクを提供することができる。
かかる実施形態の組成物は、外的な刺激によって何らかの反応を起こす材料の一種であることから、スマートマテリアルとして有用なものである。
各例の組成物を調製する際、以下に示す(P)成分、(M)成分、(R)成分をそれぞれ用いた。
化合物(P-1):熱硬化性エラストマー樹脂としてウレタンアクリレート(製品名DA-800AU、日油株式会社)を使用。硬化物のガラス転移温度マイナス30℃。
化合物(P-1)は、数平均分子量が530のポリカプロラクトンジオールと、イソホロンジイソシアネートと、2-ヒドロキシエチルアクリレートと、を反応させて得られるもの。化合物(P-1)の重量平均分子量は5200。
Fe49Co49V2(エプソンアトミックス株式会社)を使用。平均粒径8.0±1.0μm。
熱ラジカル重合開始剤として2,2’-アゾビス(2-メチルプロピオン酸)ジメチルを使用。
化合物(P-1)100質量部に対して(R)成分3質量部を添加し、撹拌によって溶解することにより、均一溶液を得た。
次いで、(M)成分を、表1に示す体積分率になるように添加し、撹拌して、粉末状の磁歪材料が分散した分散液である組成物を調製した。
体積分率は、(M)成分であるFe49Co49V2の密度を8.6g/cm3、化合物(P-1)及び(R)成分の密度を1.0g/cm3として算出した。
表1に示すように体積分率を変更した以外は、実施例1と同様にして、粉末状の磁歪材料が分散した分散液である組成物を調製した。
化合物(P-2)100質量部に対して(R)成分3質量部を添加し、撹拌によって溶解することにより、均一溶液を得た。
次いで、(M)成分を、表2に示す体積分率になるように添加し、撹拌して、粉末状の磁歪材料が分散した分散液である組成物を調製した。
体積分率は、(M)成分であるFe49Co49V2の密度を8.6g/cm3、化合物(P-2)及び(R)成分の密度を1.0g/cm3として算出した。
表2に示すように体積分率を変更した以外は、実施例5と同様にして、粉末状の磁歪材料が分散した分散液である組成物を調製した。
各例の組成物を、それぞれ、10mm×10mm×2mmの型に流し込んだ。
その後、それぞれの型をセラミックホットプレート(CHP-170DF(アズワン))上へ設置し、窒素フローしながら、80℃で2時間の熱硬化処理を行い、この後さらに、120℃で1時間の熱硬化処理を行うことにより、硬化物サンプルを得た。
図1は、本実施例における磁歪特性の評価方法を示す模式図である。
図1では、一対の電磁石10,10間に、硬化物サンプル20が配置されている。
直交型のひずみゲージ30を、硬化物サンプル20表面の6mm四方の範囲に貼付し、電磁石10によって、マイナス1テスラからプラス1テスラまでの磁場を、硬化物サンプル20表面に対して水平方向かつ一方向(z軸方向)へ印加した。尚、硬化物サンプル20表面に対して水平方向かつz軸方向に直交する方向をx軸方向としている。
その際の硬化物サンプル20の変形状態について、振動試料型磁力計を用いて評価した。かかる評価結果を、表1~2及び図2~4にそれぞれ示した。
表2の結果から、(P)成分として化合物(P-2)を用いた実施例5~8の組成物が硬化した硬化物については、いずれも「正の磁歪」を示していることが確認された。
図2中、矢印(z軸方向)は、磁場の印加方向を示している。
Claims (9)
- (P)成分:重合性基を含む化合物と、
(M)成分:粉末状の磁歪材料と、
(R)成分:ラジカル重合開始剤と、
を含有する、磁歪特性を有する組成物。 - 前記(M)成分は、鉄基磁歪合金からなる平均粒径が5μm以上50μm以下の粒子群である、請求項1に記載の組成物。
- 前記(M)成分の含有量は、前記(P)成分と前記(M)成分と前記(R)成分との合計の体積に対して、40体積%以上60体積%以下であり、
負の磁歪特性を有する、請求項1又は2に記載の組成物。 - 前記(R)成分の含有量は、前記(P)成分100質量部に対して、0.01質量部以上20質量部以下である、請求項1~3のいずれか一項に記載の組成物。
- 前記(P)成分は、重合性不飽和二重結合を含む熱硬化性樹脂である、請求項1~4のいずれか一項に記載の組成物。
- 前記(P)成分は、ガラス転移温度が-130℃以上-5℃以下の熱硬化性エラストマーである、請求項1~5のいずれか一項に記載の組成物。
- 前記熱硬化性エラストマーは、ウレタン(メタ)アクリレートである、請求項6に記載の組成物。
- 前記熱硬化性エラストマーは、数平均分子量が300以上900以下のポリカプロラクトンポリオールと、脂肪族又は脂環式ジイソシアネートと、水酸基含有(メタ)アクリレートとを反応させて得られる、重量平均分子量が2000以上30000以下のウレタン(メタ)アクリレートである、請求項7に記載の組成物。
- 請求項1~8のいずれか一項に記載の組成物が硬化した、硬化物。
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JP2019022435A (ja) * | 2017-07-12 | 2019-02-07 | 株式会社Kri | 発電ディバイス、磁気的硬質粘弾性材料の製造方法及び発電ディバイスの使用方法 |
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JP2021031516A (ja) | 2019-08-19 | 2021-03-01 | デンカ株式会社 | ゴム組成物、該ゴム組成物の加硫物及び成形品 |
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JP2005191426A (ja) * | 2003-12-26 | 2005-07-14 | Sumitomo Metal Mining Co Ltd | 高耐候性磁石粉、その製造方法及びそれを用いた希土類ボンド磁石用樹脂組成物 |
JP2008507142A (ja) * | 2004-07-17 | 2008-03-06 | カール・フロイデンベルク・カーゲー | 磁歪素子およびその使用 |
JP2017163119A (ja) | 2016-03-11 | 2017-09-14 | 国立大学法人東北大学 | 複合強化型の磁歪複合材料及びその製造方法 |
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