WO2022071294A1 - 複合体の接着信頼性及び放熱性能を評価する方法、及び複合体 - Google Patents

複合体の接着信頼性及び放熱性能を評価する方法、及び複合体 Download PDF

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Publication number
WO2022071294A1
WO2022071294A1 PCT/JP2021/035575 JP2021035575W WO2022071294A1 WO 2022071294 A1 WO2022071294 A1 WO 2022071294A1 JP 2021035575 W JP2021035575 W JP 2021035575W WO 2022071294 A1 WO2022071294 A1 WO 2022071294A1
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Prior art keywords
semi
cured product
composite
sintered body
emission intensity
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PCT/JP2021/035575
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English (en)
French (fr)
Japanese (ja)
Inventor
裕介 和久田
仁孝 南方
真也 坂口
智也 山口
厚樹 五十嵐
浩二 西村
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Denka Co Ltd
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Denka Co Ltd
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Priority to US18/246,096 priority Critical patent/US20230366829A1/en
Priority to EP21875595.7A priority patent/EP4206165A4/en
Priority to JP2022528638A priority patent/JP7257592B2/ja
Priority to CN202180062353.2A priority patent/CN116134005A/zh
Publication of WO2022071294A1 publication Critical patent/WO2022071294A1/ja
Anticipated expiration legal-status Critical
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/64—Fluorescence; Phosphorescence
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/46—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with organic materials
    • C04B41/48—Macromolecular compounds
    • C04B41/488—Other macromolecular compounds obtained otherwise than by reactions only involving unsaturated carbon-to-carbon bonds
    • C04B41/4884—Polyurethanes; Polyisocyanates
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81—Coating or impregnation
    • C04B41/82—Coating or impregnation with organic materials
    • C04B41/83—Macromolecular compounds
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/84—Systems specially adapted for particular applications
    • G01N21/8422—Investigating thin films, e.g. matrix isolation method
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/84—Systems specially adapted for particular applications
    • G01N2021/8411—Application to online plant, process monitoring
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/84—Systems specially adapted for particular applications
    • G01N21/8422—Investigating thin films, e.g. matrix isolation method
    • G01N2021/8438—Mutilayers

Definitions

  • the present disclosure relates to a method for evaluating the adhesive reliability and heat dissipation performance of a complex, and the complex.
  • thermal interface materials that have electrical insulation for electronic components or printed wiring boards. It has been used to attach it to a heat sink.
  • a composite composed of a resin and ceramics such as boron nitride is used as a heat radiating member.
  • the heat dissipation performance of the laminated body obtained by adhering the composite to other members has been evaluated for the laminated body after bonding, but it is not possible to take measures such as improving the heat dissipation performance after bonding. It's not easy.
  • the contact area between each member tends to be smaller.
  • the present inventors have conducted various studies on the intensity of fluorescence generated by irradiation of the composite with ultraviolet rays, and the adhesive performance in the laminate obtained by adhering the composite to another member. We have found that there is a correlation with heat dissipation performance, and based on this finding, we have reached the present disclosure.
  • One aspect of the present disclosure is a method for evaluating the adhesion performance and heat dissipation performance of a composite containing a porous ceramic sintered body and a semi-cured resin material filled in the pores of the ceramic sintered body. Therefore, a step of irradiating the surface of the semi-cured product of the composite with ultraviolet rays, a step of measuring the emission intensity of fluorescence generated from the semi-cured product, and adhesion of the composite using the value of the emission intensity.
  • a method including a step of evaluating performance and heat dissipation performance.
  • the method for evaluating the adhesive performance and heat dissipation performance of the composite is based on the above-mentioned new findings. Fluorescence emitted from the semi-cured product excited by ultraviolet rays is detected, and the measurement target is based on the intensity thereof. The adhesive performance and heat dissipation performance of the composite can be evaluated.
  • the cured product obtained by completely curing the semi-cured product of the composite is irradiated with ultraviolet rays, and the cured product is irradiated with ultraviolet rays.
  • the emission intensity of the fluorescence generated from the semi-cured product is X
  • the semi-cured product is irradiated with ultraviolet rays
  • the emission intensity of the fluorescence generated from the semi-cured product is Y
  • the composite is based on the value of Y / X. It may be a step of evaluating the adhesion performance and heat dissipation performance of the body.
  • the semi-cured product may contain a resin having an aromatic ring as a component. Since the semi-cured product contains a resin having an aromatic ring as a component, fluorescence is likely to be generated by irradiation with ultraviolet rays, so that the evaluation of the complex becomes easier.
  • One aspect of the present disclosure comprises a porous ceramics sintered body and a semi-cured resin material filled in the pores of the ceramics sintered body, and the semi-cured product of the composite is completely cured.
  • the cured product obtained is irradiated with ultraviolet rays
  • the emission intensity of the fluorescence generated from the cured product is X
  • the semi-cured product is irradiated with ultraviolet rays
  • the emission intensity of the fluorescence generated from the semi-cured product is Y.
  • the above-mentioned complex can exhibit excellent adhesive performance and heat dissipation when bonded to other members.
  • the semi-cured product may contain a resin having an aromatic ring as a component.
  • the present disclosure it is possible to provide an evaluation method capable of evaluating whether or not the laminated body is excellent in adhesive performance and heat dissipation performance when bonded to other members by non-destructive analysis of the composite before bonding. According to the present disclosure, it is also possible to provide a composite that can exhibit excellent adhesive performance and heat dissipation performance when bonded to other members to form a laminated body.
  • FIG. 1 is a flow chart showing a process of an evaluation method.
  • FIG. 2 is a perspective view showing an example of the complex.
  • FIG. 3 is a cross-sectional view showing an example of the laminated body.
  • each component in the composition means, when a plurality of substances corresponding to each component in the composition are present, the total amount of the plurality of substances present in the composition unless otherwise specified. ..
  • One embodiment of the method for evaluating the adhesive performance and heat dissipation performance of the composite is a composite containing a porous ceramic sintered body and a semi-cured resin material filled in the pores of the ceramic sintered body.
  • a method for evaluating the adhesion performance and heat dissipation performance of the above which is a step of irradiating the surface of the semi-cured product of the composite with ultraviolet rays, a step of measuring the emission intensity of fluorescence generated from the semi-cured product, and the emission intensity. Includes a step of evaluating the adhesion performance and heat dissipation performance of the composite using the value of. Since the evaluation method can be used to select a complex that can exhibit the adhesive performance and the heat dissipation performance in a well-balanced manner, the evaluation method can also be used for the selection method.
  • the emission intensity of fluorescence generated when the semi-cured product of the composite is irradiated with ultraviolet rays is such that the emission intensity increases due to the curing of the resin and the semi-cured product becomes tinted due to the curing of the resin. It is determined by the balance with the decrease in emission intensity due to the narrowing of the reach of ultraviolet rays due to the decrease in transparency or the decrease in transparency. More specifically, some structures (for example, structures having delocalized electrons such as carbonyl groups and aromatic rings) of the monomer component, the resin component, etc. in the semi-cured product are irradiated with ultraviolet rays. Excites electrons and causes fluorescence during their relaxation.
  • the state of the semi-cured material constituting the complex can be grasped by non-destructive inspection. Furthermore, although the reason is not always clear, the state of the semi-cured material appearing in the emission intensity of fluorescence correlates with whether or not the adhesive performance and heat dissipation performance when bonded to other members can be compatible at an appropriate level. Therefore, the above-mentioned fluorescence intensity can be used as an index for evaluating the adhesive performance and the heat dissipation performance. That is, it is possible to estimate the adhesion performance and heat dissipation after adhesion to other members based on the emission intensity of fluorescence generated from the measurement target.
  • the degree of curing in the semi-cured resin material increases, the emission intensity of fluorescence as described above tends to increase, but since there is an influence such as coloring, the degree of curing and the emission intensity of fluorescence are observed. May not always match.
  • FIG. 1 is a flow chart showing the process of the evaluation method.
  • the surface of the semi-cured product of the composite sheet is irradiated with ultraviolet rays (step S1), the emission intensity of fluorescence generated from the semi-cured product is measured (step S2), and the emission intensity is described.
  • the heat dissipation performance of the composite is evaluated using the value of (step S3).
  • step S1 the surface of the semi-cured material exposed on the surface of the complex to be measured is irradiated with ultraviolet rays.
  • the wavelength of the ultraviolet rays irradiating the semi-cured product as the excitation light may be, for example, 280 nm, 310 nm, 365 nm, 385 nm or 405 nm, but 365 nm is excellent in versatility.
  • the intensity of the ultraviolet rays irradiating the semi-cured product as the excitation light may be, for example, 0.5 mW or less.
  • the intensity of the irradiated ultraviolet rays also depends on the distance between the surface of the semi-cured product and the ultraviolet irradiation unit (UV light emitting element) that irradiates the ultraviolet rays and the sensor unit (detection element) that detects fluorescence.
  • the amount of energy) and the emission intensity of the detected fluorescence can vary. Therefore, it is assumed that this distance is fixed in the measurement. Since the emission intensity of fluorescence changes depending on the type of resin contained in the semi-cured product, for example, when the emission intensity of fluorescence is small and cannot be detected, the above distance can be shortened to increase the detection sensitivity.
  • the distance may be, for example, 35 to 300 mm or 50 to 200 mm.
  • step S2 the fluorescence generated when the electrons excited by ultraviolet rays are relaxed is detected, and the emission intensity thereof is measured.
  • the wavelength of fluorescence to be detected may be set to, for example, 280 to 405 nm.
  • the emission intensity of fluorescence the same measurement is performed on both sides of the complex to be measured, and the average value thereof is used.
  • a UV curing sensor (CUREA series manufactured by Acroedgese Co., Ltd.) or the like can be used.
  • step 3 the adhesive performance and heat dissipation performance are estimated and evaluated based on the measured fluorescence intensity.
  • the evaluation can be performed based on the correlation between the emission intensity of fluorescence measured in advance for the reference sample and the adhesion performance and heat dissipation performance when bonded to other members. For example, after measuring the emission intensity of fluorescence of one of a plurality of composite sheets cut out from the same composite, the laminate obtained by adhering to another member was completely cured with the adhesive strength and thermal resistance. The emission intensity of fluorescence in the cured product is measured, and the correlation data is acquired. Then, based on the obtained data, the adhesive performance and heat dissipation performance can be estimated and evaluated from the emission intensity of fluorescence of other complexes.
  • the evaluation can also be applied to a semi-cured resin composition having the same or similar composition.
  • a resin composition or a semi-cured product thereof is applied to and impregnated into a thinly molded ceramic sintered body, and then the cured state of the resin is adjusted by heating or the like to adjust the cured state of the resin to form a composite sheet.
  • the degree of curing of the semi-cured product in each composite sheet may vary.
  • the reference data for any one composite sheet, the fluorescence intensity is measured, and then the adhesive strength and thermal resistance of the laminate obtained by adhering to the other member are measured. (Data showing the relationship between the emission intensity of fluorescence and the adhesive performance and heat dissipation performance) obtained by measuring the above can be used to evaluate the adhesive performance and heat dissipation performance of other composite sheets.
  • Step 3 is, for example, to accumulate data acquired in advance, estimate the adhesion performance and heat dissipation performance from the emission intensity of fluorescence obtained from the complex to be measured in light of the accumulated data, and output the data. It may be evaluated using an apparatus.
  • the cured product obtained by completely curing the semi-cured product of the composite is irradiated with ultraviolet rays, and the cured product is irradiated with ultraviolet rays.
  • the emission intensity of the fluorescence generated from the semi-cured product is X
  • the semi-cured product is irradiated with ultraviolet rays
  • the emission intensity of the fluorescence generated from the semi-cured product is Y
  • the composite is based on the value of Y / X. It may be a step of evaluating the adhesion performance and heat dissipation performance of the body.
  • the complex for obtaining X is composed of a semi-cured product having the same or similar resin composition as the complex to be measured.
  • the value of Y / X is smaller than 1. If the resin constituting the semi-cured product does not become tinted and the transparency does not decrease as the curing of the resin progresses, the emission intensity of fluorescence increases as the degree of curing increases. , The value of Y / X is larger than 1.
  • the complex includes a porous ceramics sintered body and a semi-cured resin material filled in the pores of the ceramics sintered body.
  • FIG. 2 is a perspective view showing an example of the complex 10.
  • the ceramic sintered body 20 may be, for example, a nitride sintered body.
  • the nitride sintered body contains nitride particles and pores formed by sintering primary particles of nitride.
  • the cured product obtained by completely curing the semi-cured product of the composite is irradiated with ultraviolet rays, the emission intensity of fluorescence generated from the cured product is set to X, and the semi-cured product is irradiated with ultraviolet rays.
  • the emission intensity of fluorescence generated from the semi-cured product is Y
  • the value of Y / X is 3.5 to 7.0.
  • the complex for obtaining X is a complex having a semi-cured product having the same or similar resin composition as the complex to be measured as a constituent element.
  • the lower limit of the Y / X value may be, for example, 4.0 or more, or 4.3 or more. When the lower limit of the Y / X value is within the above range, the adhesive performance and heat dissipation performance when adhering to other members can be further improved.
  • the upper limit of the Y / X value may be, for example, less than 7.0, 6.3 or less, or 5.5 or less. When the upper limit of the Y / X value is within the above range, the adhesive performance and heat dissipation performance when adhering to other members can be further improved.
  • the value of Y / X can be adjusted within the above range, and may be, for example, 3.5 to 7.0, 3.5 or more and less than 7.0, 4.0 to 6.3, or the like. ..
  • the Y / X value can be controlled by adjusting the composition of the resin composition when preparing the complex and the conditions in the curing step.
  • the semi-cured product is a resin composition containing a main agent and a curing agent in which the curing reaction has partially progressed (stage B). Therefore, the semi-cured product may contain a thermosetting resin or the like produced by the reaction of the main agent and the curing agent in the resin composition.
  • the semi-cured product may contain a monomer such as a main agent and a curing agent in addition to the thermosetting resin as a resin component. It can be confirmed by, for example, a differential scanning calorimeter that the resin contained in the complex is a semi-cured product (B stage) before complete curing (C stage).
  • the semi-cured product may contain a resin having an aromatic ring as a component.
  • the semi-cured product may have, for example, at least one structural unit selected from the group consisting of a structural unit derived from a cyanate group, a structural unit derived from a bismaleimide group, and a structural unit derived from an epoxy group. ..
  • the semi-cured product of the resin composition has a structural unit derived from a cyanate group, a structural unit derived from a bismaleimide group, and a structural unit derived from an epoxy group, whereby the adhesiveness between the composite and the metal sheet is further improved. Can be improved.
  • Examples of the structural unit having a cyanate group include a triazine ring and the like.
  • Examples of the structural unit derived from the bismaleimide group include a structure represented by the following formula (1).
  • Examples of the structural unit derived from the epoxy group include a structure represented by the following general formula (2).
  • These structural units can be detected using infrared absorption spectroscopy (IR). It can be detected using proton nuclear magnetic resonance spectroscopy ( 1 H-NMR) and carbon-13 nuclear magnetic resonance spectroscopy ( 13 C-NMR). The above-mentioned structural unit may be detected by IR or 1 H-NMR and 13 C-NMR.
  • R 1 represents a hydrogen atom or other functional group.
  • the other functional group may be, for example, an alkyl group or the like.
  • the semi-cured product may contain at least one selected from the group consisting of cyanate resin, bismaleimide resin, and epoxy resin as the thermosetting resin.
  • the semi-cured product may contain, for example, a phenol resin, a melamine resin, a urea resin, an alkyd resin, or the like.
  • the semi-cured product may contain at least one curing agent selected from the group consisting of a phosphine-based curing agent and an imidazole-based curing agent.
  • the semi-cured product may be a cured product formed by curing a polymerizable compound (for example, a compound having a cyanate group, a compound having an epoxy group, etc.) contained in the resin composition with these curing agents.
  • the filling factor of the semi-cured product in the complex 10 may be, for example, 85 to 97% by volume.
  • the filling rate of the resin is within the above range, the exudation of the resin component can be sufficiently increased when the resin component is adhered to the metal sheet under heating and pressurization, and the complex 10 has more excellent adhesiveness.
  • the lower limit of the filling rate of the resin may be 88% by volume or more, 90% by volume or more, or 92% by volume or more.
  • the volume ratio of the resin in the complex 10 may be, for example, 30 to 60% by volume or 35 to 55% by volume based on the total volume of the complex 10.
  • the volume ratio of the ceramic particles constituting the ceramic sintered body 20 in the complex 10 may be, for example, 40 to 70% by volume or 45 to 65% by volume based on the total volume of the complex 10.
  • the complex 10 having such a volume ratio can achieve both excellent adhesiveness and strength at a high level.
  • the average pore diameter of the pores of the ceramic sintered body 20 may be, for example, 5 ⁇ m or less, 4 ⁇ m or less, or 3.5 ⁇ m or less. Since the size of the pores of such a ceramic sintered body 20 is small, the contact area between the particles of the ceramic particles can be sufficiently increased. Therefore, the thermal conductivity can be increased.
  • the average pore diameter of the pores of the ceramic sintered body 20 may be 0.5 ⁇ m or more, 1 ⁇ m or more, or 1.5 ⁇ m or more. Since such a ceramic sintered body 20 can be sufficiently deformed when pressed during bonding, the amount of exudation of the resin component can be increased. Therefore, the adhesiveness can be further improved.
  • the average pore diameter of the pores of the ceramic sintered body 20 can be measured by the following procedure. First, the complex 10 is heated to remove the resin. Then, using a mercury porosimeter, the pore size distribution when the ceramic sintered body 20 is pressed while increasing the pressure from 0.0042 MPa to 206.8 MPa is obtained. When the horizontal axis is the pore diameter and the vertical axis is the cumulative pore volume, the pore diameter when the cumulative pore volume reaches 50% of the total pore volume is the average pore diameter. As the mercury porosimeter, one manufactured by Shimadzu Corporation can be used.
  • the porosity of the ceramic sintered body 20, that is, the volume ratio of the pores in the ceramic sintered body 20, may be, for example, 30 to 65% by volume or 35 to 55% by volume. If the porosity becomes too large, the strength of the ceramic sintered body tends to decrease. On the other hand, if the porosity becomes too small, the amount of resin that seeps out when the composite 10 is adhered to other members tends to decrease.
  • the bulk density [B (kg / m 3 )] is calculated from the volume and mass of the ceramic sintered body 20, and the bulk density and the theoretical density of the ceramics [A (kg / m 3 )] are used. It can be obtained by the following formula (1).
  • the ceramic sintered body 20 may include at least one selected from the group consisting of boron nitride, aluminum nitride, or silicon nitride as the nitride.
  • the theoretical density A is 2280 kg / m 3 .
  • the theoretical density A is 3260 kg / m 3 .
  • the theoretical density A is 3170 kg / m 3 .
  • Porosity (% by volume) [1- (B / A)] x 100 formula (1)
  • the bulk density B may be 800 to 1500 kg / m 3 or 1000 to 1400 kg / m 3 . If the bulk density B becomes too small, the strength of the ceramic sintered body 20 tends to decrease. On the other hand, if the bulk density B becomes too large, the filling amount of the resin tends to decrease, and the amount of resin that seeps out when the composite 10 is adhered to other members tends to decrease.
  • the thickness t of the ceramic sintered body 20 may be, for example, less than 2 mm or less than 1.6 mm.
  • the pores of the ceramic sintered body 20 having such a thickness can be sufficiently filled with the resin. Therefore, the complex 10 can be miniaturized and the adhesiveness of the complex 10 can be improved.
  • Such a complex 10 is suitably used as a component of a semiconductor device. From the viewpoint of ease of manufacturing the ceramic sintered body 20, the thickness t of the ceramic sintered body 20 may be, for example, 0.1 mm or more, or 0.2 mm or more.
  • the thickness of the composite 10 may be the same as the thickness t of the ceramic sintered body 20, or may be larger than the thickness t of the ceramic sintered body 20.
  • the thickness of the complex 10 may be, for example, less than 2 mm or less than 1.6 mm.
  • the thickness of the complex 10 may be, for example, 0.1 mm or more, or 0.2 mm or more.
  • the thickness of the complex 10 is measured along the direction orthogonal to the main surfaces 10a and 10b. When the thickness of the complex 10 is not constant, the thickness may be measured by selecting arbitrary 10 points, and the average value thereof may be within the above range. Even if the thickness of the ceramic sintered body 20 is not constant, the thickness is measured by selecting arbitrary 10 points, and the average value thereof is the thickness t.
  • the sizes of the main surfaces 10a and 10b of the complex 10 are not particularly limited, and may be, for example, 500 mm 2 or more, 800 mm 2 or more, or 1000 mm 2 or more.
  • the main surface 10a and the main surface 10b of the complex 10 were quadrangular, but the shape is not limited to such a shape.
  • the main surface may be a polygon other than a quadrangle, or may be a circle.
  • the shape may be such that the corners are chamfered, or the shape may be partially cut out. Further, it may have a through hole penetrating in the thickness direction.
  • the complex as described above can be produced, for example, by the following method.
  • Examples of the method for producing the composite include a sintering step of preparing a porous ceramics sintered body, an impregnation step of impregnating the pores of the ceramics sintered body with the resin composition to obtain a resin composition impregnated body, and a resin.
  • the ceramic sintered body will be described with an example of a nitride sintered body.
  • the raw material powder used in the sintering process contains nitride.
  • the nitride contained in the raw material powder may contain, for example, at least one nitride selected from the group consisting of boron nitride, aluminum nitride, and silicon nitride.
  • the boron nitride may be amorphous boron nitride or hexagonal boron nitride.
  • the raw material powder is, for example, an amorphous boron nitride powder having an average particle size of 0.5 to 10 ⁇ m or an average particle size of 3.0 to 40 ⁇ m.
  • a certain hexagonal boron nitride powder can be used.
  • a compound containing a nitride powder may be molded and sintered to obtain a nitride sintered body. Molding may be performed by uniaxial pressurization or by a cold isotropic pressurization (CIP) method.
  • a sintering aid may be added to obtain a formulation. Examples of the sintering aid include metal oxides such as yttrium oxide, aluminum oxide and magnesium oxide, carbonates of alkali metals such as lithium carbonate and sodium carbonate, boric acid and the like.
  • the blending amount of the sintering aid is, for example, 0.01 to 20 parts by mass and 0.01 to 15 with respect to 100 parts by mass of the total of the nitride and the sintering aid. It may be parts by mass, 0.1 to 15 parts by mass, or 0.1 to 10 parts by mass.
  • the compound may be, for example, a sheet-shaped molded product by the doctor blade method.
  • the molding method is not particularly limited, and a molded product may be obtained by press molding using a mold.
  • the molding pressure may be, for example, 5 to 350 MPa.
  • the shape of the molded body is not particularly limited, and may be a block-shaped shape or a sheet-shaped shape having a predetermined thickness. When the molded body is in the form of a sheet, the operation of cutting the nitride sintered body can be omitted, and the material loss due to processing can be reduced.
  • the sintering temperature in the sintering step may be, for example, 1600 to 2200 ° C. or 1700 to 2000 ° C.
  • the sintering time may be, for example, 1 to 30 hours.
  • the atmosphere at the time of sintering may be, for example, an atmosphere of an inert gas such as nitrogen, helium, and argon.
  • a batch type furnace, a continuous type furnace, or the like can be used.
  • the batch type furnace include a muffle furnace, a tube furnace, an atmosphere furnace, and the like.
  • the continuous furnace include a rotary kiln, a screw conveyor furnace, a tunnel furnace, a belt furnace, a pusher furnace, a large continuous furnace, and the like.
  • a nitride sintered body can be obtained.
  • the nitride sintered body may be in the form of a block.
  • the nitride sintered body is in the form of a block, it is also possible to perform a cutting step of processing the nitride sintered body to a predetermined thickness.
  • the nitride sintered body is cut using, for example, a wire saw.
  • the wire saw may be, for example, a multi-cut wire saw or the like.
  • the pores of the nitride sintered body are impregnated with the resin composition to obtain a resin composition impregnated body.
  • the impregnated resin composition can be heated to start curing to adjust the viscosity.
  • the resin composition is likely to be impregnated into the inside. Further, by adjusting the degree of curing when the nitride sintered body is impregnated with the resin composition, it is suitable for impregnation and the filling rate of the resin can be sufficiently increased.
  • the temperature T3 may be, for example, 80 to 140 ° C.
  • the method of impregnation is not particularly limited, and the nitride sintered body may be immersed in the resin composition, or may be performed by applying the resin composition to the surface of the nitride sintered body.
  • the nitride sintered body can be sufficiently filled with the resin.
  • the filling rate of the resin may be, for example, 85 to 97% by volume, and the lower limit of the filling rate of the resin may be, for example, 88% by volume or more, 90% by volume or more, or 92% by volume or more.
  • the impregnation step may be performed under any conditions of reduced pressure, pressure, or atmospheric pressure. Impregnation under reduced pressure conditions, impregnation under pressurized conditions, and impregnation under atmospheric pressure may be performed in combination of two or more.
  • the pressure in the impregnation device when the impregnation step is carried out under reduced pressure conditions may be, for example, 1000 Pa or less, 500 Pa or less, 100 Pa or less, 50 Pa or less, or 20 Pa or less.
  • the pressure in the impregnation device may be, for example, 1 MPa or more, 3 MPa or more, 10 MPa or more, or 30 MPa or more.
  • the average pore diameter of the nitride sintered body may be, for example, 0.5 to 5 ⁇ m or 1 to 4 ⁇ m.
  • the resin composition for example, one that becomes the resin mentioned in the above-mentioned explanation of the complex by curing or semi-curing reaction can be used.
  • the resin composition may contain a solvent.
  • the viscosity of the resin composition may be adjusted by changing the blending amount of the solvent, or the viscosity of the resin composition may be adjusted by partially advancing the curing reaction.
  • the solvent include aliphatic alcohols such as ethanol and isopropanol, 2-methoxyethanol, 1-methoxyethanol, 2-ethoxyethanol, 1-ethoxy-2-propanol, 2-butoxyethanol and 2- (2-methoxyethoxy).
  • ketones such as ketones and hydrocarbons such as toluene and xylene. One of these may be contained alone, or two or more thereof may be contained in combination.
  • the resin composition may be thermosetting and may contain, for example, at least one compound selected from the group consisting of a compound having a cyanate group, a compound having a bismaleimide group and a compound having an epoxy group, and a curing agent. , May be contained.
  • Examples of the compound having a cyanate group include dimethylmethylenebis (1,4-phenylene) biscyanate and bis (4-cyanatephenyl) methane.
  • Dimethylmethylenebis (1,4-phenylene) biscyanate is commercially available, for example, as TACN (manufactured by Mitsubishi Gas Chemical Company, Inc., trade name).
  • Compounds having a bismaleimide group include, for example, N, N'-[(1-methylethylidene) bis [(p-phenylene) oxy (p-phenylene)]] bismaleimide, and 4,4'-diphenylmethane bismaleimide. And so on.
  • N, N'-[(1-methylethylidene) bis [(p-phenylene) oxy (p-phenylene)]] bismaleimide is commercially available, for example, as BMI-80 (manufactured by Keiai Kasei Co., Ltd., trade name). Is available.
  • Examples of the compound having an epoxy group include bisphenol F type epoxy resin, bisphenol A type epoxy resin, biphenyl type epoxy resin, and polyfunctional epoxy resin.
  • bisphenol F type epoxy resin bisphenol A type epoxy resin
  • biphenyl type epoxy resin biphenyl type epoxy resin
  • polyfunctional epoxy resin examples include 1,6-bis (2,3-epoxypropane-1-yloxy) naphthalene, which is commercially available as HP-4032D (manufactured by DIC Corporation, trade name), may be used.
  • the curing agent may contain a phosphine-based curing agent and an imidazole-based curing agent.
  • the phosphine-based curing agent can promote the triazine formation reaction by the trimerization of the compound having a cyanate group or the cyanate resin.
  • phosphine-based curing agent examples include tetraphenylphosphonium tetra-p-tolylborate and tetraphenylphosphonium tetraphenylborate.
  • Tetraphenylphosphonium tetra-p-tolylbolate is commercially available, for example, as TPP-MK (manufactured by Hokuko Chemical Industry Co., Ltd., trade name).
  • the imidazole-based curing agent produces oxazoline and promotes the curing reaction of the compound having an epoxy group or the epoxy resin.
  • Examples of the imidazole-based curing agent include 1- (1-cyanomethyl) -2-ethyl-4-methyl-1H-imidazole, 2-ethyl-4-methylimidazole and the like.
  • 1- (1-Cyanomethyl) -2-ethyl-4-methyl-1H-imidazole is commercially available, for example, as 2E4MZ-CN (manufactured by Shikoku Chemicals Corporation, trade name).
  • the content of the phosphine-based curing agent is, for example, 5 parts by mass or less, 4 parts by mass or less, or 5 parts by mass or less, based on 100 parts by mass of the total amount of the compound having a cyanate group, the compound having a bismaleimide group, and the compound having an epoxy group. It may be 3 parts by mass or less.
  • the content of the phosphine-based curing agent is, for example, 0.1 part by mass or more or 0.5 part by mass with respect to 100 parts by mass of the total amount of the compound having a cyanate group, the compound having a bismaleimide group and the compound having an epoxy group. It may be more than one part.
  • the content of the imidazole-based curing agent is, for example, 0.1 part by mass or less, 0.05 part by mass with respect to 100 parts by mass of the total amount of the compound having a cyanate group, the compound having a bismaleimide group, and the compound having an epoxy group. It may be less than a part or 0.03 part by mass or less.
  • the content of the imidazole-based curing agent is, for example, 0.001 part by mass or more, or 0.005 parts by mass with respect to 100 parts by mass of the total amount of the compound having a cyanate group, the compound having a bismaleimide group, and the compound having an epoxy group. It may be parts by mass or more.
  • the resin composition may contain components other than the main agent and the curing agent.
  • Other components further include, for example, other resins such as phenolic resins, melamine resins, urea resins, and alkyd resins, silane coupling agents, leveling agents, defoaming agents, surface modifiers, and wet dispersants. But it may be.
  • the content of these other components may be, for example, 20% by mass or less, 10% by mass or less, or 5% by mass or less, based on the total amount of the resin composition.
  • the impregnation step there is a curing step of semi-curing the resin composition impregnated in the pores.
  • the resin composition is semi-cured by heating and / or light irradiation, depending on the type of the resin composition (or the curing agent added as needed).
  • the cured state of the semi-cured product can be adjusted so that the emission intensity of fluorescence is within a predetermined range.
  • the emission intensity of fluorescence tends to increase as the curing progresses, and the emission intensity of fluorescence tends to decrease as the curing progresses beyond a certain level.
  • the composite may be bonded to the other member by temporarily crimping it to another member such as a metal sheet and then heating it.
  • the heating temperature when the resin composition is semi-cured by heating may be, for example, 80 to 130 ° C.
  • the semi-cured product obtained by semi-curing the resin composition contains, as a resin component, at least one thermosetting resin selected from the group consisting of cyanate resin, bismaleimide resin, and epoxy resin, and a curing agent. It's okay.
  • the semi-cured product contains other resins such as phenol resin, melamine resin, urea resin, and alkyd resin as resin components, as well as a silane coupling agent, a leveling agent, a defoaming agent, a surface conditioner, and a wet dispersion. It may contain a component derived from an agent or the like.
  • the surface of the semi-cured product formed in the curing step is irradiated with ultraviolet rays, and a desired composite is selected based on the emission intensity of fluorescence generated from the semi-cured product.
  • the sorting conditions can be appropriately adjusted based on the adhesive performance and heat dissipation performance required for the composite.
  • the cured product obtained by completely curing the semi-cured product of the composite is irradiated with ultraviolet rays.
  • ultraviolet rays are applied to the semi-cured product
  • Y is the emission intensity of the fluorescence generated from the semi-cured product. It may be done, and the value of Y / X may be 3.5 to 7.0.
  • FIG. 3 is a cross-sectional view when an example of the laminated body is cut in the thickness direction.
  • the laminate 100 includes a sheet-shaped composite 10, a metal sheet 30 adhered to the main surface 10a of the composite 10, and a metal sheet 40 adhered to the main surface 10b of the composite 10.
  • the metal sheets 30 and 40 may be a metal plate or a metal foil. Examples of the materials of the metal sheets 30 and 40 include aluminum and copper. The materials and thicknesses of the metal sheets 30 and 40 may be the same or different from each other. Further, it is not essential to include both the metal sheets 30 and 40, and in the modified example of the laminated body 100, only one of the metal sheets 30 and 40 may be provided.
  • the laminated body 100 may have a resin cured layer between the complex 10 and the metal sheets 30 and 40 within a range not contrary to the gist of the present disclosure.
  • the resin cured layer may be formed by additional curing of the semi-cured product exuded from the composite 10.
  • the composite 10 and the metal sheets 30 and 40 in the laminated body 100 are sufficiently firmly bonded to each other by curing the exuded semi-cured product, so that the bonding reliability is excellent.
  • the laminated body 100 is manufactured by using a sheet-shaped composite (B stage sheet) in which the above-mentioned Y / X value regarding the emission intensity of fluorescence is within a predetermined range, the laminated body 100 is also excellent in heat dissipation. Since such a laminated body is thin and has excellent adhesive reliability and heat dissipation, it can be suitably used for a semiconductor device or the like, for example, as a heat dissipation member.
  • Example 1 ⁇ Manufacturing of nitride sintered body (ceramic sintered body)> 100 parts by mass of orthoboric acid manufactured by Nippon Denko Co., Ltd. and 35 parts by mass of acetylene black (trade name: HS100) manufactured by Denka Co., Ltd. were mixed using a Henschel mixer. The obtained mixture was filled in a graphite crucible and heated in an arc furnace at 2200 ° C. for 5 hours in an argon atmosphere to obtain massive boron carbide (B 4C ). The obtained lump was coarsely pulverized with a jaw crusher to obtain a coarse powder. This coarse powder was further pulverized by a ball mill having a silicon carbide ball ( ⁇ 10 mm) to obtain pulverized powder.
  • HS100 acetylene black
  • the prepared pulverized powder was filled in a crucible made of boron nitride. Then, using a resistance heating furnace, the mixture was heated at 2000 ° C. and 0.85 MPa for 10 hours in a nitrogen gas atmosphere. In this way, a calcined product containing boron nitride (B 4 CN 4 ) was obtained.
  • a sintering aid was prepared by blending powdered boric acid and calcium carbonate. In the preparation, 50.0 parts by mass of calcium carbonate was added to 100 parts by mass of boric acid. At this time, the atomic ratio of boron to calcium was 17.5 atomic% of calcium with respect to 100 atomic% of boron. 20 parts by mass of the sintering aid was added to 100 parts by mass of the calcined product, and the mixture was mixed using a Henschel mixer to prepare a powdery compound.
  • the molded product was placed in a boron nitride container and introduced into a batch type high frequency furnace. In a batch type high frequency furnace, heating was performed under the conditions of normal pressure, nitrogen flow rate of 5 L / min, and 2000 ° C. for 5 hours. Then, the boron nitride sintered body was taken out from the boron nitride container. In this way, a sheet-shaped (square columnar) boron nitride sintered body was obtained. The thickness of the boron nitride sintered body was 1.6 mm.
  • the prepared resin composition was dropped onto the main surface of the boron nitride sintered body.
  • the dropped resin composition was spread using a rubber spatula, and the resin composition was spread over the entire main surface to obtain a resin composition-impregnated body.
  • Example 5 A complex was prepared in the same manner as in Example 1 except that the heating time in the curing step was changed to the conditions shown in Table 1.
  • the bulk density of the boron nitride sintered body and the composite is based on JIS Z 8807: 2012 "Measuring method of density and specific gravity by geometric measurement", and the length of each side of the boron nitride sintered body or the composite. It was determined based on the volume calculated from (measured by Nogis) and the mass of the boron nitride sintered body or composite measured by an electronic balance (see Section 9 of JIS Z 8807: 2012). The theoretical density of the complex was determined by the following equation (4).
  • Theoretical density of the composite true density of boron nitride sintered body + true density of semi-cured product x (1-bulk density of boron nitride sintered body / true density of boron nitride) ... Equation (4)
  • the true density of the boron nitride sintered body and the semi-cured product is based on JIS Z 8807: 2012 "Density and specific gravity measurement method by gas substitution method", and the boron nitride sintered body was measured using a dry automatic densitometer. And determined by the volume and mass of the semi-cured product (see equations (14) to (17) in Section 11 of JIS Z 8807: 2012).
  • the curing rate of the semi-cured product (semi-cured product of the resin composition) contained in the complexes prepared in Examples 1 to 5 was determined by measurement using a differential scanning calorimeter. First, the calorific value Q generated when 1 g of the uncured resin composition was completely cured was measured. Then, the temperature of the sample collected from the semi-cured product contained in the composite was raised in the same manner, and the calorific value R generated when the sample was completely cured was determined. At this time, the mass of the sample used for the measurement by the differential scanning calorimeter was the same as the resin composition used for the measurement of the calorific value Q.
  • the emission intensity of fluorescence was measured for the semi-cured product contained in the complex prepared in Examples 1 to 5.
  • Two complexes prepared in Examples 1 to 5 were prepared. One of the two prepared complexes was irradiated with ultraviolet rays, and the emission intensity of the obtained fluorescence was measured. Next, the complex was heated to further promote the curing of the semi-cured product so that the curing rate of the resin composition was 100%, and a cured product was obtained. Then, the obtained cured product was irradiated with ultraviolet rays under the same conditions as described above, and the emission intensity of the obtained fluorescence was measured. The emission intensity measured at this time was defined as X.
  • the other complex was irradiated with ultraviolet rays under the same conditions as described above, and the emission intensity of the obtained fluorescence was set to Y. Then, the value of Y / X was calculated from the value of X and the value of Y, and evaluated according to the following criteria. Even if the ratio to the value of X is calculated by using the value of the emission intensity of the fluorescence obtained before curing the semi-cured product instead of the value of Y, it corresponds well with the above Y / X. It was confirmed that it became a value.
  • the agglomerated fractured portion is the area of the portion where the composite sheet is broken, and it is shown that the larger the area ratio is, the better the adhesiveness is.
  • the present disclosure it is possible to provide an evaluation method capable of evaluating whether or not the laminated body is excellent in adhesive performance and heat dissipation performance when bonded to other members by non-destructive analysis of the composite before bonding. According to the present disclosure, it is also possible to provide a composite that can exhibit excellent adhesive performance and heat dissipation performance when bonded to other members to form a laminated body.
  • 10 complex, 10a, 10b ... main surface, 20 ... ceramic sintered body, 30, 40 ... metal sheet, 100 ... laminated body.

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