WO2018235918A1 - 樹脂材料、樹脂材料の製造方法及び積層体 - Google Patents
樹脂材料、樹脂材料の製造方法及び積層体 Download PDFInfo
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- WO2018235918A1 WO2018235918A1 PCT/JP2018/023689 JP2018023689W WO2018235918A1 WO 2018235918 A1 WO2018235918 A1 WO 2018235918A1 JP 2018023689 W JP2018023689 W JP 2018023689W WO 2018235918 A1 WO2018235918 A1 WO 2018235918A1
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- B32B9/005—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising one layer of ceramic material, e.g. porcelain, ceramic tile
- B32B9/007—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising one layer of ceramic material, e.g. porcelain, ceramic tile comprising carbon, e.g. graphite, composite carbon
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Definitions
- the present invention relates to a resin material containing inorganic particles and a binder resin, and a method of producing the resin material.
- the present invention also relates to a laminate provided with an insulating layer containing inorganic particles and a binder resin.
- a ceramic substrate having high thermal conductivity As one means for solving the above-mentioned problems, there is a means using a ceramic substrate having high thermal conductivity as a heat dissipation substrate on which a power semiconductor device or the like is mounted.
- An alumina substrate, an aluminum nitride substrate, etc. are mentioned as such a ceramic substrate.
- a resin composition using boron nitride having a low coefficient of linear expansion, particularly hexagonal boron nitride has attracted attention as a heat dissipation material.
- the crystal structure of hexagonal boron nitride is a layered structure of a hexagonal network similar to graphite, and the particle shape of hexagonal boron nitride is scaly.
- hexagonal boron nitride has a property that the thermal conductivity in the plane direction is higher than the thermal conductivity in the thickness direction, and the thermal conductivity is anisotropic.
- the said resin composition may be used as a heat conductive sheet or a prepreg.
- Patent Document 1 discloses a thermally conductive sheet in which a part or all of boron nitride particles are dispersed in a thermosetting resin in the form of aggregated particles.
- the thermally conductive sheet further contains metal oxide particles.
- the total content of the metal oxide particles and the boron nitride particles is 40% by volume to 70% by volume.
- the volume ratio of the metal oxide particles to the boron nitride particles is 10:90 to 50:50.
- the median diameter of the metal oxide particles is 0.5 ⁇ m to 30 ⁇ m.
- Patent Document 2 discloses a prepreg for heat and pressure molding, in which a thermosetting resin composition containing an inorganic filler of two or more components is in a sheet-like and semi-cured state.
- the inorganic filler is an aggregate of primary particles, and includes the filler (1) having an average particle diameter d1 of 10 ⁇ m or more and 70 ⁇ m or less.
- the inorganic filler is in the form of particles, and includes the filler (2) in which the average particle diameter d2 of the particles is 0.1 ⁇ m to 30 ⁇ m.
- the content of the filler (1) is 5% by volume to 40% by volume in a total of 100% by volume of the thermosetting resin solid content and the inorganic filler.
- the content of the filler (2) is 10% by volume to 50% by volume in a total of 100% by volume of the thermosetting resin solid content and the inorganic filler.
- the total content of the inorganic filler in 20% by volume of the thermosetting resin composition is 20% by volume to 80% by volume.
- the conventional heat conductive sheet containing boron nitride like patent document 1, 2 etc. may be laminated
- a circuit pattern may be formed by treating the copper foil by etching or the like.
- the first inorganic particle includes a first inorganic particle having an average aspect ratio of 2 or less, a second inorganic particle having an average aspect ratio of more than 2 and a binder resin.
- the absolute value of the difference between the average particle diameter of the second inorganic particles and the average particle diameter of the second inorganic particles is 10 .mu.m or less, and the average particle diameter of the first inorganic particles is 1 .mu.m or more and less than 20 .mu.m.
- the average major axis of the inorganic particles is 2 ⁇ m or more, and the content of the second inorganic particles exceeds 40% by volume in a total of 100% by volume of the first inorganic particles and the second inorganic particles.
- a resin material is provided.
- the resin material contains 50% by volume or less of the first inorganic particles in a total of 100% by volume of the first inorganic particles and the second inorganic particles.
- the material of the first inorganic particle contains an aluminum element or a carbon element.
- the average circularity of the first inorganic particles is 0.9 or more.
- the second inorganic particle is included as part of aggregated particles.
- the average aspect ratio of the second inorganic particles is 15 or less.
- the material of the second inorganic particle is boron nitride.
- the thermal conductivity of the first inorganic particle and the thermal conductivity of the second inorganic particle are each 10 W / m ⁇ K or more.
- the binder resin contains a thermosetting compound and a thermosetting agent.
- the resin material is a resin sheet.
- a method for producing a resin material as described above wherein the first inorganic particles having an average aspect ratio of 2 or less and the second inorganic particles having an average aspect ratio exceeding 2
- a method of producing a resin material comprising the step of blending the binder resin.
- a heat conductor an insulating layer laminated on one surface of the heat conductor, and a conductive layer laminated on the surface of the insulating layer opposite to the heat conductor
- the first insulating particle includes a first inorganic particle having an average aspect ratio of 2 or less, a second inorganic particle having an average aspect ratio exceeding 2 and a binder resin, and the first inorganic particle
- the absolute value of the difference between the average particle diameter of the second inorganic particles and the average particle diameter of the second inorganic particles is 10 .mu.m or less, and the average particle diameter of the first inorganic particles is 1 .mu.m or more and less than 20 .mu.m.
- the average major axis of the inorganic particles is 2 ⁇ m or more, and the content of the second inorganic particles exceeds 40% by volume in a total of 100% by volume of the first inorganic particles and the second inorganic particles.
- a laminate is provided.
- the resin material according to the present invention includes a first inorganic particle having an average aspect ratio of 2 or less, a second inorganic particle having an average aspect ratio of more than 2, and a binder resin.
- the absolute value of the difference between the average particle size of the first inorganic particles and the average major axis of the second inorganic particles is 10 ⁇ m or less
- the average particles of the first inorganic particles are The diameter is 1 ⁇ m or more and less than 20 ⁇ m
- the average major axis of the second inorganic particles is 2 ⁇ m or more.
- the content of the second inorganic particles exceeds 40 volume% in a total of 100 volume% of the first inorganic particles and the second inorganic particles.
- the adhesiveness can be effectively enhanced, and the long-term insulation reliability can be effectively enhanced.
- a laminate according to the present invention comprises a thermal conductor, an insulating layer laminated on one surface of the thermal conductor, and a conductive layer laminated on the surface of the insulating layer opposite to the thermal conductor.
- the insulating layer includes a first inorganic particle having an average aspect ratio of 2 or less, a second inorganic particle having an average aspect ratio of more than 2, and a binder resin.
- the absolute value of the difference between the average particle diameter of the first inorganic particles and the average major axis of the second inorganic particles is 10 ⁇ m or less, and the average particles of the first inorganic particles are The diameter is 1 ⁇ m or more and less than 20 ⁇ m, and the average major axis of the second inorganic particles is 2 ⁇ m or more.
- the content of the second inorganic particles exceeds 40 volume% in a total of 100 volume% of the first inorganic particles and the second inorganic particles.
- FIG. 1 is a cross-sectional view schematically showing a laminate obtained using a resin material according to an embodiment of the present invention.
- the resin material according to the present invention includes a first inorganic particle having an average aspect ratio of 2 or less, a second inorganic particle having an average aspect ratio of more than 2, and a binder resin.
- the resin material according to the present invention contains a plurality of first inorganic particles.
- the resin material according to the present invention contains a plurality of second inorganic particles.
- the absolute value of the difference between the average particle size of the first inorganic particles and the average major axis of the second inorganic particles is 10 ⁇ m or less.
- the average particle diameter of the first inorganic particles is 1 ⁇ m or more and less than 20 ⁇ m.
- the average major axis of the second inorganic particles is 2 ⁇ m or more.
- the content of the second inorganic particles exceeds 40 volume% in a total of 100 volume% of the first inorganic particles and the second inorganic particles.
- the average particle size of the first inorganic particles can be determined by averaging the particle sizes of the entire first inorganic particles having an average aspect ratio of 2 or less.
- the average major axis of the second inorganic particles is determined by averaging the major axes of the entire second inorganic particles having an average aspect ratio of more than 2.
- the resin material according to the present invention is obtained by blending the first inorganic particles, the second inorganic particles, and the binder resin.
- a laminate according to the present invention comprises a thermal conductor, an insulating layer laminated on one surface of the thermal conductor, and a conductive layer laminated on the surface of the insulating layer opposite to the thermal conductor.
- the insulating layer contains a first inorganic particle having an average aspect ratio of 2 or less, a second inorganic particle having an average aspect ratio of more than 2, and a binder resin.
- the insulating layer contains a plurality of first inorganic particles.
- the insulating layer contains a plurality of second inorganic particles.
- the absolute value of the difference between the average particle size of the first inorganic particles and the average major axis of the second inorganic particles is 10 ⁇ m or less.
- the average particle diameter of the first inorganic particles is 1 ⁇ m or more and less than 20 ⁇ m.
- the average major axis of the second inorganic particles is 2 ⁇ m or more.
- the content of the second inorganic particles exceeds 40 volume% in a total of 100 volume% of the first inorganic particles and the second inorganic particles.
- the resin material according to the present invention and the laminate according to the present invention are provided with the above-described configuration, so that the adhesiveness can be effectively enhanced, and the long-term insulation reliability can be effectively enhanced.
- the resin material according to the present invention may be used as a resin sheet.
- a laminate in which a conductive layer such as copper foil is laminated on a first surface of a resin sheet in the case of a laminate, the resin sheet is an insulating layer
- the form of peeling when peeling occurs between the resin sheet and the conductive layer Observed.
- the second inorganic particles oriented in the plane direction in the region near the first surface of the resin sheet are broken or peeled off, thereby peeling within the region near the first surface of the resin sheet
- the present inventors have found that may occur.
- the second inorganic particles in the region near the first surface of the resin sheet, not only the second inorganic particles having a relatively large aspect ratio but also the first aspect having a relatively small aspect ratio Of inorganic particles.
- the second inorganic particles when a conductive layer such as a heat conductor or copper foil is laminated on a resin sheet and a laminate is produced by pressing or the like, the second inorganic particles The orientation is controlled in the thickness direction by the first inorganic particles. For this reason, since content of the 2nd inorganic particle orientated to the surface direction can be decreased, it can be made hard to produce peeling in the 1st surface near field area of a resin sheet.
- the second inorganic particles oriented in the thickness direction function as anchors, thereby making it difficult to cause peeling of the resin sheet in the region near the first surface.
- the adhesion between the resin sheet and the conductive layer such as copper foil can be further effectively enhanced.
- the absolute value of the difference between the average particle diameter of the first inorganic particles and the average major diameter of the second inorganic particles is relatively large. The smaller one is preferable. If the average particle diameter of the first inorganic particles is relatively larger than the average major diameter of the second inorganic particles, the second inorganic particles will be disposed around the first inorganic particles, and the thickness It becomes difficult to control the orientation of the second inorganic particles in the direction.
- the average particle size of the first inorganic particles is relatively smaller than the average major axis of the second inorganic particles, the first inorganic particles will be disposed between the second inorganic particles, It becomes difficult to control the orientation of the second inorganic particles in the longitudinal direction.
- the orientation of the second inorganic particles is controlled in the thickness direction in the region near the first surface of the resin sheet, and the heat in the thickness direction
- the conductivity can be increased.
- boron nitride when used as the second inorganic particle, boron nitride has such a property that the thermal conductivity in the plane direction is higher than the thermal conductivity in the thickness direction and the thermal conductivity is anisotropic. As it has, by controlling the orientation of boron nitride, the thermal conductivity in the thickness direction can be more effectively enhanced.
- a circuit pattern may be formed by processing the copper foil which is a conductive layer by an etching etc.
- partial discharge may occur between the peeled circuit pattern and the outer surface of the laminate, the laminate may be deteriorated, and long-term insulation reliability may be lowered.
- the resin material according to the present invention and the laminate according to the present invention since the adhesiveness between the resin sheet and the conductive layer such as copper foil can be enhanced as described above, the formed circuit pattern is peeled off from the laminate It is possible to prevent long-term insulation reliability more effectively.
- the resin material according to the present invention and the laminate according to the present invention include the first inorganic particles.
- the first inorganic particles preferably have an insulating property.
- the first inorganic particles are preferably insulating particles.
- the first inorganic particle is, for example, an inorganic filler. At least one type of inorganic particle is used as the first inorganic particle.
- As the first inorganic particles only one type of inorganic particles may be used, or two or more types of inorganic particles may be used in combination. Two or more types of inorganic particles may be blended to constitute the first inorganic particle.
- the inorganic particles formed of a certain material and the inorganic particles formed of a material different from the certain material may be mixed to constitute the first inorganic particles.
- the average aspect ratio of the first inorganic particles is 2 or less.
- the lower limit of the average aspect ratio of the first inorganic particles is not particularly limited.
- the average aspect ratio of the first inorganic particles may be 1 or more.
- the aspect ratio of the first inorganic particle indicates a major axis / a minor axis.
- the aspect ratio of the first inorganic particle can be obtained by observing an arbitrarily selected first inorganic particle with an electron microscope or an optical microscope and measuring the major axis / minor axis of each inorganic particle.
- the average aspect ratio can be determined by averaging the aspect ratios of arbitrary 50 first inorganic particles.
- the average aspect ratio of any 50 first inorganic particles is approximately equal to the average aspect ratio of the first inorganic particles as a whole.
- the particle diameter of the first inorganic particle is preferably 1 ⁇ m or more.
- the particle diameter of the first inorganic particle means a diameter when the inorganic particles are spherical, and when the inorganic particles have a shape other than spherical, it is assumed to be a spherical equivalent of the volume of the inorganic particles. Means the diameter at the time of
- the average particle diameter of the first inorganic particles is 1 ⁇ m or more and less than 20 ⁇ m.
- the average particle diameter of the first inorganic particles is preferably more than 6 ⁇ m, more preferably 7 ⁇ m or more, from the viewpoint of more effectively improving the adhesiveness and the viewpoint of more effectively enhancing the long-term insulation reliability.
- Preferably it is 18 micrometers or less, More preferably, it is 15 micrometers or less.
- the average particle size of the first inorganic particles is preferably an average particle size obtained by averaging particle sizes on a volume basis.
- the average particle diameter of the first inorganic particles is preferably the particle diameter (d50) of the first inorganic particles when the cumulative volume of the first inorganic particles is 50%.
- the average particle diameter of the first inorganic particles can be measured using a “laser diffraction type particle size distribution measuring device” manufactured by Horiba, Ltd.
- the average particle diameter of the first inorganic particles is obtained by observing 50 arbitrarily selected first inorganic particles with an electron microscope or an optical microscope, measuring the particle diameter of each inorganic particle, and calculating the average value. It can also be determined by The average particle size of any 50 first inorganic particles is approximately equal to the average particle size of the first inorganic particles as a whole.
- the average circularity of the first inorganic particles is preferably 0.70 or more, more preferably 0, from the viewpoint of more effectively improving the adhesiveness and the viewpoint of enhancing the long-term insulation reliability more effectively. And 80 or more, preferably 1.00 or less.
- the circularity of the first inorganic particle is determined by cutting an optionally selected first inorganic particle from an electron microscopic image of a cross section of a laminate prepared by mixing the first inorganic particle and a thermosetting resin or the like.
- the area (S) and the perimeter (L) can be measured and calculated by the following equation (1).
- the degree of circularity is a value representing the likeness of a circle, and means that as the degree of circularity approaches one, it becomes closer to a circle.
- Circularity [4 ⁇ S / L 2 ] Equation (1)
- the average circularity of the first inorganic particles is preferably 0.90 or more because the effects of the present invention can be exhibited effectively.
- the average circularity of the first inorganic particles may exceed 0.90.
- the average circularity of the first inorganic particles is determined by averaging the circularities of the entire first inorganic particles having an average aspect ratio of 2 or less.
- the average circularity of the first inorganic particles can be determined by averaging the circularities of the 50 arbitrarily selected first inorganic particles.
- the average circularity of any 50 first inorganic particles is approximately equal to the average circularity over the first inorganic particles.
- the first inorganic particles are preferably spherical particles or rounded particles.
- the first inorganic particles may be spherical particles or rounded particles.
- the spherical particles mean particles having the circularity of 0.95 or more.
- rounded particles mean particles having a rounded shape overall and having few crystal corners, and specifically mean particles having the above-mentioned circularity of 0.70 or more and 0.90 or less. Do.
- the first inorganic particles are spherical particles, the flowability of the resin material can be effectively improved.
- the first inorganic particles are round particles, the thermal conductivity of the resin material and the laminate can be effectively improved.
- spherical particles may be used as the first inorganic particles, or only rounded particles may be used, and spherical particles and rounded particles And may be used in combination.
- the material of the first inorganic particle is not particularly limited. It is preferable that the said 1st inorganic particle is an insulating filler.
- the material of the first inorganic particle may not be boron nitride.
- Examples of the material of the first inorganic particle include metal oxides such as aluminum oxide (alumina), calcium oxide and magnesium oxide, metal nitrides such as aluminum nitride and titanium nitride, aluminum hydroxide, and hydroxide Metal hydroxides such as magnesium, metal salts of carbonates such as calcium carbonate and magnesium carbonate, metal salts of silicates such as calcium silicate, hydrated metal compounds, crystalline silica, non-crystalline silica, boron nitride, silicon carbide, And diamonds.
- the material of the first inorganic particle only one type may be used, or two or more types may be used in combination.
- the material of the first inorganic particle preferably contains an aluminum element or a carbon element.
- the material of the first inorganic particle is preferably aluminum oxide (alumina), aluminum nitride, aluminum hydroxide or diamond More preferably, it is aluminum oxide (alumina) or diamond. These preferred materials may be used alone or in combination of two or more.
- the thermal conductivity of the first inorganic particle is preferably 10 W / m ⁇ K or more, more preferably 20 W / m ⁇ K or more.
- the upper limit of the thermal conductivity of the first inorganic particle is not particularly limited.
- the thermal conductivity of the first inorganic particle may be 300 W / m ⁇ K or less, and may be 200 W / m ⁇ K or less.
- the first inorganic particles are contained in 100% by volume of the resin material and 100% by volume of the insulating layer.
- the content is preferably 5% by volume or more, more preferably 10% by volume or more, preferably 35% by volume or less, more preferably 30% by volume or less.
- the first inorganic particles and the second inorganic particles in the resin material and the insulating layer are contained in 50% by volume or less, more preferably 40% by volume or less, in the total 100% by volume of the above.
- the lower limit of the content of the first inorganic particles is not particularly limited in the total 100% by volume of the first inorganic particles and the second inorganic particles.
- the content of the first inorganic particles in the total of 100% by volume of the first inorganic particles and the second inorganic particles may be 10% by volume or more, or even 20% by volume or more. Good.
- the resin material according to the present invention and the laminate according to the present invention include the second inorganic particles. It is preferable that the said 2nd inorganic particle has insulation.
- the second inorganic particles are preferably insulating particles. It is preferable that the said 2nd inorganic particle is an insulating filler. At least one type of inorganic particle is used as the second inorganic particle. As the second inorganic particles, only one type of inorganic particles may be used, or two or more types of inorganic particles may be used in combination. Two or more types of inorganic particles may be blended to constitute the second inorganic particle.
- An inorganic particle formed of a certain material and an inorganic particle formed of a material different from the certain material may be mixed to constitute the second inorganic particle.
- the average aspect ratio of the second inorganic particles is more than 2.
- the average aspect ratio of the second inorganic particles is preferably 4 or more, more preferably 5 or more, from the viewpoint of more effectively improving the adhesiveness and the viewpoint of enhancing the long-term insulation reliability more effectively. Preferably it is 15 or less, More preferably, it is 12 or less.
- the second inorganic particle is, for example, a plate-like filler. In the present specification, plate-like fillers are also included in the particles.
- the aspect ratio of the second inorganic particle indicates a major axis / a minor axis.
- the aspect ratio of the second inorganic particles is obtained by observing the cross section of a sheet or a laminate prepared by mixing the second inorganic particles and a curable resin and curing the mixture with an electron microscope or an optical microscope. It can be determined by measuring the major axis / minor axis of the inorganic particles.
- the average aspect ratio can be determined by averaging the aspect ratios of arbitrary 50 second inorganic particles. The average aspect ratio of any 50 second inorganic particles is approximately equal to the average aspect ratio of the second inorganic particles as a whole.
- the particle diameter of the second inorganic particle is preferably 1 ⁇ m or more.
- the particle diameter of the second inorganic particles is preferably the major diameter.
- the average major axis of the second inorganic particles is 2 ⁇ m or more.
- the average major axis of the second inorganic particles is preferably 3 ⁇ m or more, more preferably 5 ⁇ m or more, from the viewpoint of more effectively improving the adhesiveness and the viewpoint of enhancing the long-term insulation reliability more effectively.
- it is 40 micrometers or less, More preferably, it is 20 micrometers or less.
- the average major axis of the second inorganic particles is obtained by observing 50 arbitrarily selected second inorganic particles with an electron microscope or an optical microscope, measuring the major axis of the second inorganic particles, and calculating the average value. It can be determined by The average major axis of any 50 second inorganic particles is approximately equal to the average major axis of the entire second inorganic particles.
- the average major axis of the second inorganic particles is arbitrary by observing the cross section of a sheet or a laminate prepared by mixing the second inorganic particles and a curable resin and curing the mixture with an electron microscope or an optical microscope. It can also be determined by measuring the major diameter of the 50 second inorganic particles selected in the above and calculating the average value.
- the absolute value of the difference between the average particle diameter of the first inorganic particles and the average major diameter of the second inorganic particles is 10 ⁇ m or less. From the viewpoint of more effectively improving the adhesiveness and the viewpoint of more effectively enhancing the long-term insulation reliability, the difference between the average particle diameter of the first inorganic particles and the average major diameter of the second inorganic particles
- the absolute value of is preferably 0 ⁇ m or more, more preferably 1 ⁇ m or more, preferably 7 ⁇ m or less, more preferably 5 ⁇ m or less.
- the second inorganic particle is contained as a part of the aggregated particles.
- the resin material according to the present invention and the laminate according to the present invention may contain agglomerated particles, and may contain primary particles constituting agglomerated particles as the second inorganic particles.
- the said 2nd inorganic particle is a primary particle which comprises an aggregation particle.
- the second inorganic particles are preferably not aggregated particles.
- a boron nitride aggregation particle etc. are mentioned, for example.
- the average major axis means the average major axis of the primary particles.
- the material of the second inorganic particle is preferably boron nitride from the viewpoint of more effectively improving the adhesiveness and the viewpoint of more effectively enhancing the long-term insulation reliability. It does not specifically limit as said boron nitride.
- the boron nitride include hexagonal boron nitride, cubic boron nitride, boron nitride produced by a reduction nitriding method of a boron compound and ammonia, boron nitride produced from a boron compound and a nitrogen-containing compound such as melamine, and And boron nitride produced from sodium borohydride and ammonium chloride.
- the boron nitride is preferably hexagonal boron nitride.
- the thermal conductivity of the second inorganic particle is preferably 10 W / m ⁇ K or more, more preferably 30 W / m ⁇ K or more. Since the second inorganic particles have a relatively large aspect ratio and may have anisotropy in thermal conductivity, the thermal conductivity of the second inorganic particles is preferably an average thermal conductivity.
- the upper limit of the thermal conductivity of the second inorganic particle is not particularly limited.
- the thermal conductivity of the second inorganic particle may be 300 W / m ⁇ K or less, and may be 200 W / m ⁇ K or less.
- the second inorganic particles are contained in 100% by volume of the resin material and 100% by volume of the insulating layer.
- the content is preferably 25% by volume or more, more preferably 30% by volume or more, preferably 60% by volume or less, and more preferably 55% by volume or less.
- the content of the second inorganic particles is more than 40% by volume in 100% by volume of the total of the first inorganic particles and the second inorganic particles. From the viewpoint of more effectively improving the adhesiveness and the viewpoint of more effectively enhancing the long-term insulation reliability, the first inorganic particles and the second inorganic particles in 100% by volume in total
- the content of the inorganic particles of 2 is preferably 45% by volume or more, more preferably 50% by volume or more, and still more preferably 60% by volume or more.
- the first inorganic particles and the second inorganic particles in 100% by volume in total
- the content of the inorganic particles of 2 is preferably 90% by volume or less, more preferably 80% by volume or less.
- the resin material according to the present invention and the laminate according to the present invention may contain inorganic particles (third inorganic particles) having a particle diameter of less than 1 ⁇ m.
- the resin material according to the present invention and the laminate according to the present invention may contain the third inorganic particles as the first inorganic particles, and include the third inorganic particles as the second inorganic particles.
- the third inorganic particles may be included as the first inorganic particles and the second inorganic particles. From the viewpoint of more effectively improving the adhesiveness and the viewpoint of more effectively enhancing the long-term insulation reliability, the resin material and the laminate preferably include the third inorganic particles.
- the third inorganic particles may be aggregated particles or primary particles constituting the aggregated particles.
- the material of the third inorganic particle is not particularly limited. As a material of the said 3rd inorganic particle, the material of the said 1st inorganic particle mentioned above, the material of the said 2nd inorganic particle, etc. are mentioned.
- the first inorganic particles, the second inorganic particles, and the third inorganic particles may be surface-treated with a surface treatment agent such as a silane coupling agent.
- the particle diameter of the third inorganic particle is preferably less than 1 ⁇ m.
- the particle diameter of the third inorganic particle can be determined by the method of calculating the particle diameter of the first inorganic particle or the particle diameter of the second inorganic particle described above.
- the content of the third inorganic particles is not particularly limited. From the viewpoint of more effectively improving the thermal conductivity, the content of the third inorganic particles is preferably 0.5% by volume or more in 100% by volume of the resin material and 100% by volume of the insulating layer. More preferably, it is 1% by volume or more, preferably 5% by volume or less, and more preferably 3% by volume or less.
- the resin material according to the present invention and the laminate according to the present invention include a binder resin.
- the binder resin is not particularly limited.
- the binder resin a known insulating resin is used.
- the binder resin preferably contains a thermoplastic component (thermoplastic compound) or a curable component, and more preferably contains a curable component.
- a thermosetting component and a photocurable component are mentioned.
- the said thermosetting component contains a thermosetting compound and a thermosetting agent.
- the said photocurable component contains a photocurable compound and a photoinitiator.
- the binder resin preferably contains a thermosetting component.
- the said binder resin contains a thermosetting compound and a thermosetting agent.
- the thermosetting component may contain a curing accelerator.
- the binder resin may contain a curing accelerator.
- the binder resin may be used alone or in combination of two or more.
- thermosetting compound is not specifically limited.
- examples of the thermosetting compound include styrene compounds, phenoxy compounds, oxetane compounds, epoxy compounds, episulfide compounds, (meth) acrylic compounds, phenol compounds, amino compounds, unsaturated polyester compounds, polyurethane compounds, silicone compounds, and polyimide compounds. It can be mentioned. Only one type of the thermosetting compound may be used, or two or more types may be used in combination.
- the thermosetting compound preferably contains an epoxy compound.
- the epoxy compound is an organic compound having at least one epoxy group.
- the epoxy compounds may be used alone or in combination of two or more.
- epoxy compounds examples include bisphenol A type epoxy compounds, bisphenol F type epoxy compounds, bisphenol S type epoxy compounds, phenol novolac type epoxy compounds, biphenyl type epoxy compounds, biphenyl novolac type epoxy compounds, biphenol type epoxy compounds, naphthalene type epoxy compounds , Fluorene type epoxy compounds, phenol aralkyl type epoxy compounds, naphthol aralkyl type epoxy compounds, dicyclopentadiene type epoxy compounds, anthracene type epoxy compounds, epoxy compounds having an adamantane skeleton, epoxy compounds having a tricyclodecane skeleton, naphthalene ether type
- skeleton, etc. are mentioned.
- the said epoxy compound is a bisphenol A-type epoxy compound from a viewpoint of improving adhesiveness more effectively, and a viewpoint of improving long-term insulation reliability more effectively.
- the content of the thermosetting compound is preferably 20% by volume in 100% by volume of the resin material.
- the amount is more preferably 25% by volume or more, preferably 80% by volume or less, and more preferably 70% by volume or less.
- the content of the component derived from the thermosetting compound is preferably contained in 100% by volume of the insulating layer. Is 20 volume% or more, more preferably 25 volume% or more, preferably 80 volume% or less, more preferably 70 volume% or less.
- thermosetting agent heat curing agent
- the thermosetting agent which can harden the above-mentioned thermosetting compound
- the thermal curing agent includes a curing catalyst. Only one type of thermosetting agent may be used, or two or more types may be used in combination.
- thermosetting agent cyanate ester compound (cyanate ester curing agent), phenol compound (phenol heat curing agent), amine compound (amine heat curing agent), thiol compound (thiol heat curing agent), imidazole compound, phosphine compound, There may be mentioned acid anhydrides, active ester compounds and dicyandiamide.
- the thermosetting agent preferably has a functional group capable of reacting with the epoxy group of the epoxy compound.
- novolak-type cyanate ester resin novolak-type cyanate ester resin, bisphenol-type cyanate ester resin, the prepolymer by which these were partially trimerized, etc.
- the novolac type cyanate ester resin include phenol novolac type cyanate ester resin and alkylphenol type cyanate ester resin.
- bisphenol type cyanate ester resin bisphenol A type cyanate ester resin, bisphenol E type cyanate ester resin, tetramethyl bisphenol F type cyanate ester resin, etc. are mentioned.
- cyanate ester compounds include phenol novolac type cyanate ester resins ("PT-30” and “PT-60” manufactured by Lonza Japan Co., Ltd.), and prepolymers in which bisphenol type cyanate ester resins are trimerized (Lonza Japan Company-made “BA-230S”, “BA-3000S”, “BTP-1000S” and “BTP-6020S” etc. are mentioned.
- phenol compound examples include novolac type phenol, biphenol type phenol, naphthalene type phenol, dicyclopentadiene type phenol, aralkyl type phenol and dicyclopentadiene type phenol.
- novolac type phenol (“TD-2091” manufactured by DIC Corporation), biphenyl novolac type phenol (“MEHC-7851” manufactured by Meiwa Kasei Co., Ltd.), aralkyl type phenol compound (“MEH manufactured by Meiwa Chemical Co., Ltd.”
- phenol having an aminotriazine skeleton (“LA1356” and “LA3018-50P” manufactured by DIC Corporation).
- the content of the total of the thermosetting compound and the thermosetting agent in 100% by volume of the resin material is preferably 20% by volume or more, more preferably 25% by volume or more, and preferably 50% by volume or less. More preferably, it is 45 volume% or less.
- the total content of components derived from the thermosetting compound and the thermosetting agent in 100 volume% of the insulating layer is preferably 20 volume% or more, more preferably 25 volume% or more, and preferably 50 It is at most volume%, more preferably at most 45 volume%. When the total content is the above lower limit and the above upper limit, the thermal conductivity can be more effectively enhanced, and the adhesiveness can be more effectively enhanced.
- the content ratio of the thermosetting compound to the thermosetting agent is appropriately selected so that the thermosetting compound is cured.
- the content of the thermosetting agent is appropriately selected so that the thermosetting compound cures well.
- the content of the thermosetting agent is preferably 1 part by weight or more, more preferably 3 parts by weight or more, preferably 50 parts by weight or less, more preferably 30 parts by weight, based on 100 parts by weight of the thermosetting compound. Part or less. It becomes much easier to fully harden a thermosetting compound as content of the above-mentioned thermosetting agent is more than the above-mentioned minimum.
- the content of the thermosetting agent is less than or equal to the upper limit, it is difficult to generate an excess of thermosetting agent that does not contribute to curing. For this reason, the heat resistance and adhesiveness of hardened
- the said resin material may contain other components generally used for resin sheets, such as a hardening accelerator, a dispersing agent, a chelating agent, antioxidant, and a curable sheet other than the component mentioned above.
- the said resin material may contain the polymer component in order to improve the moldability of resin sheets etc.
- a polyimide etc. are mentioned as said polymer component.
- the said resin material may contain the solvent. From the viewpoint of further suppressing the generation of voids in the resin sheet or the like, the content of the solvent in 100% by weight of the resin material is preferably 5% by weight or less.
- the resin material may be a paste or a curable paste.
- the resin material may be a resin sheet or a curable sheet.
- a cured product can be obtained by curing the resin material.
- the cured product is a cured product of the resin material, and is formed of the resin material.
- the resin material may be produced by laminating two or more resin sheets.
- one or more layers of the resin sheet having two or more layers may be the resin material according to the present invention.
- the method for producing the resin material includes the step of blending the first inorganic particles, the second inorganic particles, and the binder resin.
- a method of blending the first inorganic particles, the second inorganic particles, and the binder resin can be a conventionally known mixing method, and is not particularly limited.
- Examples of a method of blending the first inorganic particles, the second inorganic particles, and the binder resin include a method of kneading using a homodisper stirrer.
- a layered product concerning the present invention is provided with a heat conductor, an insulating layer, and a conductive layer.
- the insulating layer is laminated on one surface of the heat conductor.
- the conductive layer is laminated on the surface of the insulating layer opposite to the heat conductor.
- the insulating layer may be laminated also on the other surface of the heat conductor.
- the material of the insulating layer is the above-described resin material.
- the insulating layer is preferably a cured product of the above-described resin material. The cured product may be obtained by heating and pressing the resin material using a press or the like.
- the heat conductivity of the heat conductor is preferably 10 W / m ⁇ K or more.
- An appropriate heat conductor can be used as the above-mentioned heat conductor. It is preferable to use a metal material as the heat conductor. As said metal material, metal foil, a metal plate, etc. are mentioned.
- the heat conductor is preferably the metal foil or the metal plate, and more preferably the metal plate.
- the material of the metal material is preferably aluminum, copper or gold, and more preferably aluminum or copper.
- the metal for forming the said conductive layer is not specifically limited.
- the metal include gold, silver, palladium, copper, platinum, zinc, iron, tin, lead, aluminum, cobalt, indium, nickel, chromium, titanium, antimony, bismuth, thallium, germanium, cadmium, silicon, tungsten , Molybdenum, and alloys thereof.
- tin-doped indium oxide (ITO), a solder, etc. are mentioned as said metal. From the viewpoint of more effectively improving the thermal conductivity, aluminum, copper or gold is preferable, and aluminum or copper is more preferable.
- the method for forming the conductive layer is not particularly limited.
- a method of forming the said conductive layer the method by electroless-plating, the method by electroplating, the method of thermocompression-bonding the said insulating layer and metal foil, etc. are mentioned, for example. Since the formation of the conductive layer is simple, a method of heat-pressing the insulating layer and the metal foil is preferable.
- FIG. 1 is a cross-sectional view schematically showing a laminate obtained using a resin material according to an embodiment of the present invention.
- FIG. 1 for convenience of illustration, the actual size and thickness are different.
- the laminate 1 shown in FIG. 1 includes an insulating layer 2, a conductive layer 3, and a heat conductor 4.
- the insulating layer 2, the conductive layer 3 and the heat conductor 4 are the above-mentioned insulating layer, conductive layer and heat conductor.
- Insulating layer 2 has one surface (first surface) 2a and the other surface (second surface) 2b.
- the conductive layer 3 has one surface (first surface) 3a and the other surface (second surface) 3b.
- the heat conductor 4 has one surface (first surface) 4a and the other surface (second surface) 4b.
- the conductive layer 3 is stacked on the one surface (first surface) 2 a side of the insulating layer 2.
- the heat conductor 4 is laminated on the other surface (second surface) 2 b side of the insulating layer 2.
- the insulating layer 2 is stacked on the other surface (second surface) 3 b side of the conductive layer 3.
- the insulating layer 2 is laminated on the side of one surface (first surface) 4 a of the heat conductor 4.
- An insulating layer 2 is disposed between the conductive layer 3 and the heat conductor 4.
- the manufacturing method of the said laminated body is not specifically limited.
- Examples of the method for producing the laminate include a method in which the heat conductor, the insulating layer, and the conductive layer are stacked, and heat compression bonding is performed using a vacuum press or the like.
- the pressing may not necessarily be vacuum.
- the insulating layer 2 includes the first inorganic particles 11 having an average aspect ratio of 2 or less, the second inorganic particles 12 having an average aspect ratio of more than 2, and the cured product portion 13. And.
- the first inorganic particles 11 and the second inorganic particles 12 are the first inorganic particles and the second inorganic particles described above.
- the binder resin contains a thermosetting compound and a thermosetting agent.
- the cured product portion 13 is a portion where the binder resin is cured.
- the cured product portion 13 is obtained by curing the binder resin.
- the cured product portion 13 may be a portion obtained by curing a thermosetting resin and a binder resin containing a thermosetting agent.
- the laminate can be used in various applications where high thermal conductivity and mechanical strength are required.
- the said laminated body is arrange
- the laminate is used as a radiator of a power card installed between a CPU and a fin, or an inverter of an electric car.
- the laminate can be used as an insulating circuit substrate.
- Binder resin thermosetting compound: (1) "Epicoat 828US” manufactured by Mitsubishi Chemical Corporation, epoxy compound (2) “NC-3000” manufactured by Nippon Kayaku Co., Ltd., epoxy compound (3) "HP-4032D” manufactured by DIC, naphthalene type epoxy compound
- Binder resin thermosetting agent: (1) "Dicyandiamide” manufactured by Tokyo Chemical Industry Co., Ltd. (2) “2 MZA-PW” manufactured by Shikoku Kasei Kogyo Co., Ltd., an isocyanuric-modified solid dispersion type imidazole (3) a cyanate ester compound-containing liquid (“BA-3000 S” manufactured by Lonza Japan Co., Ltd., solid content 75 wt% The solid content was described in the blending amount.))
- Binder resin (hardening accelerator): (1) Imidazole compound (2-phenyl-4-methylimidazole, "2P4MZ” manufactured by Shikoku Kasei Kogyo Co., Ltd., anionic curing accelerator)
- Inorganic particles (1) Showa Denko “AS-50”, average particle diameter 9 ⁇ m, average aspect ratio 1.2 (average aspect ratio is 2 or less), average circularity 0.78, thermal conductivity 30 W / m ⁇ K, oxidation Aluminum (2) Micron Corporation “AX10-75”, average particle diameter 8 ⁇ m, average aspect ratio 1.0 (average aspect ratio is 2 or less), average circularity 0.99, thermal conductivity 30 W / m ⁇ K, oxidation Aluminum (3) Showa Denko “CB-P05”, average particle diameter 4 ⁇ m, average aspect ratio 1.0 (average aspect ratio is 2 or less), average circularity 0.99, thermal conductivity 30 W / m ⁇ K, Aluminum oxide (4) Showa Denko CB-P15, average particle diameter 16 ⁇ m, average aspect ratio 1.0 (average aspect ratio is 2 or less), average circularity 0.99, thermal conductivity 30 W / m ⁇ K , Oxidized aluminum (5) Showa Denko "CB-A30S”, average particle diameter 28 ⁇ m, average aspect ratio
- PTX60 average major axis 7 ⁇ m, average aspect ratio 12 (average aspect ratio is more than 2), thermal conductivity 60 W / m ⁇ K, boron nitride aggregated particles (8) Showa Denko “UHP-G1H", Inc. "UHP-G1H", average major axis 4 ⁇ m, average aspect ratio 7 (average aspect ratio is more than 2), thermal conductivity 60 W / m ⁇ K, boron nitride aggregated particles (9) Mizushima Alloy Iron Co., Ltd.
- HP-40 average major axis 7 ⁇ m, average aspect ratio 7 (average aspect ratio over 2), thermal conductivity 60 W / m ⁇ K, boron nitride agglomerated particles (10) manufactured by Momentive" PT110 ", average major axis 45 ⁇ m, Average aspect ratio 9.5 (average aspect ratio exceeds 2), thermal conductivity 60 W / m ⁇ K, boron nitride (11) manufactured by Momentive "PT100", average major axis 13 ⁇ m, average aspect ratio 16 (average aspect ratio 2), thermal conductivity 60 W / m ⁇ K, boron nitride (12) “CMM5-10 manufactured by Tomei Diamond Co., Ltd., average particle diameter 5.5 ⁇ m, average aspect ratio 1.3 (average aspect ratio is 2 or less) ), Average circularity 0.73, thermal conductivity 2000 W / m ⁇ K, diamond
- the average aspect ratio of the inorganic particles was measured as follows.
- Method of measuring the average aspect ratio of inorganic particles The cross section of the sheet or laminate prepared by mixing and curing the inorganic particles and the curable resin is observed with an electron microscope or an optical microscope, and the length / short diameter of each of 50 arbitrarily selected inorganic particles is It measured and calculated
- Method of measuring the average particle size of the first inorganic particles The value of the particle diameter (d50) of the first inorganic particles when the cumulative volume of the first inorganic particles was 50% was measured using a “laser diffraction type particle size distribution measuring device” manufactured by Horiba, Ltd. .
- Method of measuring the average major axis of the second inorganic particles The cross section of the sheet or laminate prepared by mixing and curing the second inorganic particles and the curable resin is observed with an electron microscope or an optical microscope, and the major diameter of 50 arbitrarily selected second inorganic particles The average value was calculated.
- the absolute value of the difference between the average particle diameter of the first inorganic particles and the average major diameter of the second inorganic particles was calculated from the average particle diameter of the first inorganic particles and the average major diameter of the second inorganic particles obtained. .
- Thermal Conductivity The obtained laminate was cut into 1 cm square, and carbon black was sprayed on both sides to prepare a measurement sample. The thermal conductivity was calculated by the laser flash method using the obtained measurement sample. Thermal conductivity calculated the relative value which set the value of comparative example 1 to 1.0, and judged it on the basis of the following.
- the obtained laminate was cut into a size of 50 mm ⁇ 120 mm to obtain a test sample.
- the copper foil was peeled off so that the copper foil with a center width of 10 mm of the obtained test sample remained, and the peel strength of the copper foil was measured according to JIS C 6481 with respect to the copper foil with a center width of 10 mm.
- a peel strength measuring apparatus a "Tensilon universal tester" manufactured by Orientec Co., Ltd. was used.
- the peel strength of the copper foil was measured for 20 test samples.
- the average value of the peel strength measurement values of the copper foils in the 20 test samples was taken as the 90 degree peel strength.
- the 90-degree peel strength was determined based on the following criteria by calculating a relative value with the value of Comparative Example 1 being 1.0.
- Dielectric breakdown strength By etching the copper foil in the obtained laminate, the copper foil was patterned into a circle having a diameter of 2 cm to obtain a test sample. An alternating voltage was applied between the test samples at a temperature of 25 ° C. using a withstand voltage tester (“MODEL7473” manufactured by ETECH Electronics) so that the voltage was increased at a rate of 0.33 kV / sec. The voltage at which a current of 10 mA flowed through the test sample was taken as the breakdown voltage. The breakdown voltage was normalized by dividing it by the thickness of the test sample to calculate the breakdown strength. The dielectric breakdown strength was determined based on the following criteria.
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Abstract
Description
本発明に係る樹脂材料は、平均アスペクト比が2以下である第1の無機粒子と、平均アスペクト比が2を超える第2の無機粒子と、バインダー樹脂とを含む。本発明に係る樹脂材料は、第1の無機粒子を複数個含む。本発明に係る樹脂材料は、第2の無機粒子を複数個含む。
本発明に係る樹脂材料及び本発明に係る積層体は、第1の無機粒子を含む。上記第1の無機粒子は、絶縁性を有することが好ましい。上記第1の無機粒子は、絶縁性粒子であることが好ましい。上記第1の無機粒子は、例えば、無機フィラーである。上記第1の無機粒子として、少なくとも1種類の無機粒子が用いられる。上記第1の無機粒子として、1種類の無機粒子のみが用いられてもよく、2種類以上の無機粒子が併用されてもよい。2種類以上の無機粒子が配合されて、第1の無機粒子が構成されてもよい。ある材料により形成された無機粒子と、上記ある材料とは異なる材料により形成された無機粒子とが混合されて、第1の無機粒子が構成されてもよい。
本発明に係る樹脂材料及び本発明に係る積層体は、第2の無機粒子を含む。上記第2の無機粒子は、絶縁性を有することが好ましい。上記第2の無機粒子は、絶縁性粒子であることが好ましい。上記第2の無機粒子は、絶縁性フィラーであることが好ましい。上記第2の無機粒子として、少なくとも1種類の無機粒子が用いられる。上記第2の無機粒子として、1種類の無機粒子のみが用いられてもよく、2種類以上の無機粒子が併用されてもよい。2種類以上の無機粒子が配合されて、第2の無機粒子が構成されてもよい。ある材料により形成された無機粒子と、上記ある材料とは異なる材料により形成された無機粒子とが混合されて、第2の無機粒子が構成されてもよい。
本発明に係る樹脂材料及び本発明に係る積層体では、粒子径が1μm未満の無機粒子(第3の無機粒子)を含んでいてもよい。本発明に係る樹脂材料及び本発明に係る積層体では、上記第1の無機粒子として上記第3の無機粒子を含んでいてもよく、上記第2の無機粒子として上記第3の無機粒子を含んでいてもよく、上記第1の無機粒子及び上記第2の無機粒子として上記第3の無機粒子を含んでいてもよい。接着性をより一層効果的に高める観点、及び長期絶縁信頼性をより一層効果的に高める観点からは、上記樹脂材料及び上記積層体は、上記第3の無機粒子を含むことが好ましい。上記第3の無機粒子は、凝集粒子であってもよく、凝集粒子を構成する一次粒子であってもよい。上記第3の無機粒子の材料は特に限定されない。上記第3の無機粒子の材料としては、上述した上記第1の無機粒子の材料及び上記第2の無機粒子の材料等が挙げられる。
本発明に係る樹脂材料及び本発明に係る積層体は、バインダー樹脂を含む。上記バインダー樹脂は特に限定されない。上記バインダー樹脂としては、公知の絶縁性の樹脂が用いられる。上記バインダー樹脂は、熱可塑性成分(熱可塑性化合物)又は硬化性成分を含むことが好ましく、硬化性成分を含むことがより好ましい。上記硬化性成分としては、熱硬化性成分及び光硬化性成分が挙げられる。上記熱硬化性成分は、熱硬化性化合物及び熱硬化剤を含むことが好ましい。上記光硬化性成分は、光硬化性化合物及び光重合開始剤を含むことが好ましい。上記バインダー樹脂は、熱硬化性成分を含むことが好ましい。上記バインダー樹脂は、熱硬化性化合物と熱硬化剤とを含むことが好ましい。上記熱硬化性成分は、硬化促進剤を含んでいてもよい。上記バインダー樹脂は、硬化促進剤を含んでいてもよい。上記バインダー樹脂は、1種のみが用いられてもよく、2種以上が併用されてもよい。
本発明に係る樹脂材料及び本発明に係る積層体では、上記熱硬化性化合物とともに熱硬化剤を用いることが好ましい。上記熱硬化剤は特に限定されない。上記熱硬化剤として、上記熱硬化性化合物を硬化させることができる熱硬化剤を適宜用いることができる。また、本明細書において、熱硬化剤には、硬化触媒が含まれる。熱硬化剤は、1種のみが用いられてもよく、2種以上が併用されてもよい。
上記樹脂材料は、上述した成分の他に、硬化促進剤、分散剤、キレート剤、酸化防止剤等の樹脂シート、及び硬化性シートに一般に用いられる他の成分を含んでいてもよい。また、上記樹脂材料は、樹脂シート等の成形性を向上させるためにポリマー成分を含んでいてもよい。上記ポリマー成分としては、ポリイミド等が挙げられる。また、上記樹脂材料は、溶剤を含んでいてもよい。樹脂シート等におけるボイドの発生をより一層抑制する観点からは、上記樹脂材料100重量%中の上記溶剤の含有量は、5重量%以下であることが好ましい。
上記樹脂材料は、ペーストであってもよく、硬化性ペーストであってもよい。上記樹脂材料は、樹脂シートであってもよく、硬化性シートであってもよい。上記樹脂材料が硬化性成分を含む場合には、上記樹脂材料を硬化させることにより硬化物を得ることができる。上記硬化物は、上記樹脂材料の硬化物であり、上記樹脂材料により形成されている。
本発明に係る積層体は、熱伝導体と、絶縁層と、導電層とを備える。上記絶縁層は、上記熱伝導体の一方の表面に積層されている。上記導電層は、上記絶縁層の上記熱伝導体とは反対側の表面に積層されている。上記熱伝導体の他方の表面にも、上記絶縁層が積層されていてもよい。本発明に係る積層体では、上記絶縁層の材料は、上述した樹脂材料である。本発明に係る積層体では、上記絶縁層は、上述した樹脂材料の硬化物であることが好ましい。上記硬化物は、上記樹脂材料をプレス等を用いて加熱及び加圧処理をすることにより得られてもよい。
上記熱伝導体の熱伝導率は、好ましくは10W/m・K以上である。上記熱伝導体としては、適宜の熱伝導体を用いることができる。上記熱伝導体は、金属材を用いることが好ましい。上記金属材としては、金属箔及び金属板等が挙げられる。上記熱伝導体は、上記金属箔又は上記金属板であることが好ましく、上記金属板であることがより好ましい。
上記導電層を形成するための金属は特に限定されない。上記金属としては、例えば、金、銀、パラジウム、銅、白金、亜鉛、鉄、錫、鉛、アルミニウム、コバルト、インジウム、ニッケル、クロム、チタン、アンチモン、ビスマス、タリウム、ゲルマニウム、カドミウム、ケイ素、タングステン、モリブデン及びこれらの合金等が挙げられる。また、上記金属としては、錫ドープ酸化インジウム(ITO)及びはんだ等が挙げられる。熱伝導性をより一層効果的に高める観点からは、アルミニウム、銅又は金であることが好ましく、アルミニウム又は銅であることがより好ましい。
(1)三菱化学社製「エピコート828US」、エポキシ化合物
(2)日本化薬社製「NC-3000」、エポキシ化合物
(3)DIC社製「HP-4032D」、ナフタレン型エポキシ化合物
(1)東京化成工業社製「ジシアンジアミド」
(2)四国化成工業社製「2MZA-PW」、イソシアヌル変性固体分散型イミダゾール
(3)シアネートエステル化合物含有液(ロンザジャパン社製「BA-3000S」、固形分75重量%(下記の表に示す配合量には固形分量を記載した。))
(1)イミダゾール化合物(2-フェニル-4-メチルイミダゾール、四国化成工業社製「2P4MZ」、アニオン性硬化促進剤)
(1)昭和電工社製「AS-50」、平均粒子径9μm、平均アスペクト比1.2(平均アスペクト比は2以下)、平均円形度0.78、熱伝導率30W/m・K、酸化アルミニウム
(2)マイクロン社製「AX10-75」、平均粒子径8μm、平均アスペクト比1.0(平均アスペクト比は2以下)、平均円形度0.99、熱伝導率30W/m・K、酸化アルミニウム
(3)昭和電工社製「CB-P05」、平均粒子径4μm、平均アスペクト比1.0(平均アスペクト比は2以下)、平均円形度0.99、熱伝導率30W/m・K、酸化アルミニウム
(4)昭和電工社製「CB-P15」、平均粒子径16μm、平均アスペクト比1.0(平均アスペクト比は2以下)、平均円形度0.99、熱伝導率30W/m・K、酸化アルミニウム
(5)昭和電工社製「CB-A30S」、平均粒子径28μm、平均アスペクト比1.0(平均アスペクト比は2以下)、平均円形度0.99、熱伝導率30W/m・K、酸化アルミニウム
(6)アドマテックス社製「AO-502」、平均粒子径0.7μm、平均アスペクト比1.0(平均アスペクト比は2以下)、平均円形度0.98、熱伝導率30W/m・K、酸化アルミニウム
(7)モメンティブ社製「PTX60」、平均長径7μm、平均アスペクト比12(平均アスペクト比は2を超える)、熱伝導率60W/m・K、窒化ホウ素凝集粒子
(8)昭和電工社製「UHP-G1H」、平均長径4μm、平均アスペクト比7(平均アスペクト比は2を超える)、熱伝導率60W/m・K、窒化ホウ素凝集粒子
(9)水島合金鉄社製「HP-40」、平均長径7μm、平均アスペクト比7(平均アスペクト比は2を超える)、熱伝導率60W/m・K、窒化ホウ素凝集粒子
(10)モメンティブ社製「PT110」、平均長径45μm、平均アスペクト比9.5(平均アスペクト比は2を超える)、熱伝導率60W/m・K、窒化ホウ素
(11)モメンティブ社製「PT100」、平均長径13μm、平均アスペクト比16(平均アスペクト比は2を超える)、熱伝導率60W/m・K、窒化ホウ素
(12)「トーメイダイヤモンド社製「CMM5-10」、平均粒子径5.5μm、平均アスペクト比1.3(平均アスペクト比は2以下)、平均円形度0.73、熱伝導率2000W/m・K、ダイヤモンド
無機粒子の平均アスペクト比を以下のようにして測定した。
無機粒子と硬化性樹脂とを混合し、硬化させて作製したシート又は積層体の断面を電子顕微鏡又は光学顕微鏡にて観察し、任意に選択された50個の各無機粒子の長径/短径を測定し、平均値を算出することにより求めた。
(1)樹脂材料の作製
下記の表1~3に示す成分を下記の表1~3に示す配合量で配合し、遊星式攪拌機を用いて500rpmで25分間攪拌することにより、樹脂材料を得た。
得られた樹脂材料を離型PETシート(厚み50μm)上に、厚み350μmになるように塗工し、90℃のオーブン内で10分間乾燥して硬化性シート(絶縁層)を形成した。その後、離型PETシートを剥がして、硬化性シート(絶縁層)の両面を、銅箔とアルミニウム板とで挟み、温度200℃、圧力12MPaの条件で真空プレスすることにより積層体を作製した。
(1)第1の無機粒子及び第2の無機粒子の有無
得られた樹脂材料において、第1の無機粒子及び第2の無機粒子が配合されているか否かを確認した。第1の無機粒子及び第2の無機粒子の有無を以下の基準で判定した。
○:樹脂材料中に、第1の無機粒子及び第2の無機粒子が配合されている
×:樹脂材料中に、第1の無機粒子又は第2の無機粒子が配合されていない
第1の無機粒子の平均粒子径及び第2の無機粒子の平均長径を以下のようにして測定した。
堀場製作所社製「レーザー回折式粒度分布測定装置」を用いて測定し、第1の無機粒子の累積体積が50%であるときの第1の無機粒子の粒子径(d50)の値を算出した。
第2の無機粒子と硬化性樹脂とを混合し、硬化させて作製したシート又は積層体の断面を電子顕微鏡又は光学顕微鏡にて観察し、任意に選択した50個の第2の無機粒子の長径を測定し、平均値を算出した。
得られた積層体を1cm角にカットした後、両面にカーボンブラックをスプレーすることで測定サンプルを作製した。得られた測定サンプルを用いて、レーザーフラッシュ法により熱伝導率を算出した。熱伝導率は、比較例1の値を1.0とした相対値を算出し、以下の基準で判定した。
○○:熱伝導率が1.5以上
○:熱伝導率が1.0を超え1.5未満
△:比較例1(1.0)
×:熱伝導率が1.0未満
得られた積層体を50mm×120mmの大きさに切り出して、テストサンプルを得た。得られたテストサンプルの中央幅10mmの銅箔が残るように銅箔を剥がし、中央幅10mmの銅箔に対して、JIS C 6481に準拠して、銅箔の引きはがし強さを測定した。ピール強度測定装置としては、オリエンテック社製「テンシロン万能試験機」を用いた。20個のテストサンプルについて、銅箔の引きはがし強さを測定した。20個のテストサンプルにおける銅箔の引きはがし強さの測定値の平均値を、90度ピール強度とした。90度ピール強度は、比較例1の値を1.0とした相対値を算出し、以下の基準で判定した。
○:90度ピール強度が1.0を超える
△:比較例1(1.0)
×:90度ピール強度が1.0未満
得られた積層体における銅箔をエッチングすることにより、直径2cmの円形に銅箔をパターニングして、テストサンプルを得た。耐電圧試験機(ETECH Electronics社製「MODEL7473」)を用いて、テストサンプル間に0.33kV/秒の速度で電圧が上昇するように、温度25℃にて交流電圧を印加した。テストサンプルに10mAの電流が流れた電圧を絶縁破壊電圧とした。絶縁破壊電圧をテストサンプルの厚みで除算することで規格化し、絶縁破壊強度を算出した。絶縁破壊強度を以下の基準で判定した。
○○:60kV/mm以上
○:30kV/mm以上60kV/mm未満
×:30kV/mm未満
上記の(5)と同様にして、20個のテストサンプルを得た。得られた20個のテストサンプルを用いて、テストサンプル間に3kVの交流電圧を、温度85℃及び湿度85%の環境下で1000時間印加して、絶縁破壊が発生するか否かを評価した。長期絶縁信頼性を以下の基準で判定した。
○:絶縁破壊が発生したテストサンプルが0個
△:絶縁破壊が発生したテストサンプルが1個以上10個未満
×:絶縁破壊が発生したテストサンプルが10個以上
2…絶縁層
2a…一方の表面(第1の表面)
2b…他方の表面(第2の表面)
3…導電層
3a…一方の表面(第1の表面)
3b…他方の表面(第2の表面)
4…熱伝導体
4a…一方の表面(第1の表面)
4b…他方の表面(第2の表面)
11…第1の無機粒子
12…第2の無機粒子
13…硬化物部(バインダー樹脂が硬化した部分)
Claims (12)
- 平均アスペクト比が2以下である第1の無機粒子と、平均アスペクト比が2を超える第2の無機粒子と、バインダー樹脂とを含み、
前記第1の無機粒子の平均粒子径と前記第2の無機粒子の平均長径との差の絶対値が、10μm以下であり、
前記第1の無機粒子の平均粒子径が、1μm以上20μm未満であり、
前記第2の無機粒子の平均長径が、2μm以上であり、
前記第1の無機粒子と前記第2の無機粒子との合計100体積%中、前記第2の無機粒子の含有量が、40体積%を超える、樹脂材料。 - 前記第1の無機粒子と前記第2の無機粒子との合計100体積%中、前記第1の無機粒子を50体積%以下で含む、請求項1に記載の樹脂材料。
- 前記第1の無機粒子の材料が、アルミニウム元素又は炭素元素を含む、請求項1又は2に記載の樹脂材料。
- 前記第1の無機粒子の平均円形度が、0.9以上である、請求項1~3のいずれか1項に記載の樹脂材料。
- 前記第2の無機粒子が、凝集粒子の一部として含まれている、請求項1~4のいずれか1項に記載の樹脂材料。
- 前記第2の無機粒子の平均アスペクト比が、15以下である、請求項1~5のいずれか1項に記載の樹脂材料。
- 前記第2の無機粒子の材料が、窒化ホウ素である、請求項1~6のいずれか1項に記載の樹脂材料。
- 前記第1の無機粒子の熱伝導率と前記第2の無機粒子の熱伝導率とがそれぞれ、10W/m・K以上である、請求項1~7のいずれか1項に記載の樹脂材料。
- 前記バインダー樹脂が、熱硬化性化合物と熱硬化剤とを含む、請求項1~8のいずれか1項に記載の樹脂材料。
- 樹脂シートである、請求項1~9のいずれか1項に記載の樹脂材料。
- 請求項1~10のいずれか1項に記載の樹脂材料の製造方法であって、
平均アスペクト比が2以下である前記第1の無機粒子と、平均アスペクト比が2を超える前記第2の無機粒子と、前記バインダー樹脂とを配合する工程を備える、樹脂材料の製造方法。 - 熱伝導体と、前記熱伝導体の一方の表面に積層された絶縁層と、前記絶縁層の前記熱伝導体とは反対側の表面に積層された導電層とを備え、
前記絶縁層が、平均アスペクト比が2以下である第1の無機粒子と、平均アスペクト比が2を超える第2の無機粒子と、バインダー樹脂とを含み、
前記第1の無機粒子の平均粒子径と前記第2の無機粒子の平均長径との差の絶対値が、10μm以下であり、
前記第1の無機粒子の平均粒子径が、1μm以上20μm未満であり、
前記第2の無機粒子の平均長径が、2μm以上であり、
前記第1の無機粒子と前記第2の無機粒子との合計100体積%中、前記第2の無機粒子の含有量が、40体積%を超える、積層体。
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