WO2021201012A1 - 複合体の製造方法 - Google Patents

複合体の製造方法 Download PDF

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Publication number
WO2021201012A1
WO2021201012A1 PCT/JP2021/013655 JP2021013655W WO2021201012A1 WO 2021201012 A1 WO2021201012 A1 WO 2021201012A1 JP 2021013655 W JP2021013655 W JP 2021013655W WO 2021201012 A1 WO2021201012 A1 WO 2021201012A1
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Prior art keywords
boron nitride
sintered body
nitride sintered
resin
complex
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Ceased
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PCT/JP2021/013655
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English (en)
French (fr)
Japanese (ja)
Inventor
仁孝 南方
裕介 和久田
真也 坂口
智也 山口
西村　浩二
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Denka Co Ltd
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Denka Co Ltd
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Priority to JP2022512575A priority Critical patent/JP7510497B2/ja
Priority to US17/906,890 priority patent/US20230141729A1/en
Priority to EP21779621.8A priority patent/EP4112588B1/en
Priority to CN202180022026.4A priority patent/CN115298151B/zh
Publication of WO2021201012A1 publication Critical patent/WO2021201012A1/ja
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K2201/00—Indexing scheme relating to printed circuits covered by H05K1/00
    • H05K2201/06—Thermal details

Definitions

  • This disclosure relates to a method for producing a complex.
  • thermal interface materials that have electrical insulation properties for electronic components or printed wiring boards. It has been used to attach it to a heat sink.
  • a composite heat dissipation member composed of a resin and ceramics such as boron nitride is used.
  • Patent Document 1 proposes a technique for reducing the anisotropy of thermal conductivity while having excellent thermal conductivity by setting the degree of orientation and the graphitization index within a predetermined range.
  • the present disclosure provides a production method capable of producing a complex having excellent insulating properties.
  • the present disclosure comprises, in one aspect, a sintering step of forming and heating a formulation containing boron nitride powder and a sintering aid to obtain a boron nitride sintered body containing boron nitride particles and pores.
  • a composite having a boron nitride sintered body and a resin filled in at least a part of the pores of the boron nitride sintered body, which comprises an impregnation step of impregnating the boron nitride sintered body with a resin composition. Provide a manufacturing method.
  • a boron nitride sintered body is obtained by molding and heating a compound containing boron nitride and a sintering aid.
  • the pore diameter of the pores contained in this boron nitride sintered body is sufficiently small. Therefore, in the impregnation step, the pores can be sufficiently impregnated with the resin composition by the capillary phenomenon. Therefore, a complex having sufficiently reduced voids can be produced. Since such a complex has excellent electrical insulation, it is useful as, for example, a heat radiating member of an electronic component. However, the application is not limited to the heat radiating member.
  • the present disclosure includes a nitriding step of calcining boron carbide powder in a nitrogen atmosphere to obtain a calcined product containing boron nitride, and molding and heating of a formulation containing the calcined product and a sintering aid.
  • a method for producing a composite comprising a resin filled in at least a part of the pores of a boron sintered body.
  • a boron nitride sintered body is obtained by molding and heating a calcined product containing boron nitride and a compound containing a sintering aid.
  • the pore diameter of the pores contained in this boron nitride sintered body is sufficiently small. Therefore, in the impregnation step, the pores can be sufficiently impregnated with the resin composition by the capillary phenomenon. Therefore, a complex having sufficiently reduced voids can be produced. Since such a complex has excellent electrical insulation, it is useful as, for example, a heat radiating member of an electronic component. However, the application is not limited to the heat radiating member.
  • the porosity of the boron nitride sintered body obtained in the sintering step may be 30 to 65% by volume. Thereby, the balance between the mass and the strength of the complex can be preferably maintained.
  • the boron nitride sintered body obtained in the sintering step has a thickness of 2 mm or more, and the boron nitride sintered body is cut between the sintering step and the impregnation step to form a sheet having a thickness of less than 2 mm. It may have a cutting step to obtain a boron nitride sintered body. By processing the sheet in this way, a complex having a high resin filling rate can be obtained. Such a complex is more excellent in electrical insulation.
  • the thickness of the boron nitride sintered body obtained in the sintering step is less than 2 mm, and in the impregnation step, the resin composition may be impregnated without cutting the boron nitride sintered body obtained in the sintering step. As a result, it is possible to suppress the generation of chips generated by cutting and increase the yield of the complex.
  • the impregnation step there may be a curing step of curing the resin filled in the pores of the boron nitride sintered body.
  • FIG. 1 is a perspective view showing an example of a composite and a boron nitride sintered body.
  • the production method of the present embodiment includes a nitriding step of calcining boron carbide powder in a nitrogen-pressurized atmosphere to obtain a calcined product containing boron nitride, molding of a compound containing the calcined product and a sintering aid, and It has a sintering step of obtaining a boron nitride sintered body containing boron nitride particles and pores by heating, and an impregnation step of impregnating the boron nitride sintered body with a resin composition.
  • Boron carbide powder can be prepared, for example, by the following procedure. After mixing boric acid and acetylene black, the mixture is heated at 1800 to 2400 ° C. for 1 to 10 hours in an inert gas atmosphere to obtain a boron carbide mass.
  • the boron carbide mass can be prepared by pulverizing, washing, removing impurities, and drying.
  • the boron carbide powder is calcined in a nitrogen atmosphere to obtain a calcined product containing boron nitride (B 4 CN 4).
  • the firing temperature in the nitriding step may be 1800 ° C. or higher, and may be 1900 ° C. or higher. Further, the firing temperature may be 2400 ° C. or lower, and may be 2200 ° C. or lower. The firing temperature may be, for example, 1800 to 2400 ° C.
  • the pressure in the nitriding step may be 0.6 MPa or more, and may be 0.7 MPa or more. Further, the pressure may be 1.0 MPa or less, and may be 0.9 MPa or less. The pressure may be, for example, 0.6 to 1.0 MPa. If the pressure is too low, nitriding of boron carbide tends to be difficult to proceed. On the other hand, if the pressure is too high, the manufacturing cost tends to increase.
  • the pressure in the present disclosure is an absolute pressure.
  • the nitrogen gas concentration in the nitrogen atmosphere in the nitriding step may be 95% by volume or more, and may be 99.9% by volume or more.
  • the partial pressure of nitrogen may be in the pressure range described above.
  • the firing time in the nitriding step is not particularly limited as long as the nitriding proceeds sufficiently, and may be, for example, 6 to 30 hours or 8 to 20 hours.
  • a calcined product containing boron nitride particles obtained in the nitriding step and a sintering aid may be blended to obtain a compound.
  • the sintering aid may contain a boron compound and a calcium compound.
  • the compound may contain 1 to 30 parts by mass in total of the boron compound and the calcium compound with respect to 100 parts by mass of the fired product. With such a content, while suppressing the excessive grain growth of the primary particles, the grain growth is moderately promoted to promote sintering, and the primary particles of boron nitride are firmly and closely adhered to each other over a wide area. Join.
  • the formulation may contain a total of 2 to 30 parts by mass of the boron compound and the calcium compound with respect to 100 parts by mass of the calcined product, and may contain 5 to 25 parts by mass. It may contain 8 to 20 parts by mass.
  • the formulation may contain 0.5 to 40 atomic% of calcium constituting a calcium compound, or 0.7 to 30 atomic%, based on 100 atomic% of boron constituting the boron compound.
  • Examples of the boron compound include boric acid, boron oxide, borax and the like.
  • Examples of the calcium compound include calcium carbonate and calcium oxide.
  • the sintering aid may contain components other than boric acid and calcium carbonate. Examples of such a component include carbonates of alkali metals such as lithium carbonate and sodium carbonate.
  • a binder may be added to the compound. Examples of the binder include an acrylic compound and the like.
  • the fired product may be crushed using a general crusher or crusher.
  • a ball mill, a Henschel mixer, a vibration mill, a jet mill and the like can be used.
  • "crushing” also includes “crushing”.
  • the calcined product may be crushed and then the sintering aid may be blended, or the calcined product and the sintering aid may be blended and then pulverized and mixed at the same time.
  • the compound may be a block-shaped molded product by powder pressing or die molding, or may be a sheet-shaped molded product by the doctor blade method.
  • the molding pressure may be, for example, 5 to 350 MPa.
  • the shape of the molded product is preferably, for example, a sheet having a thickness of 2 mm or less. If the boron nitride sintered body is manufactured using such a sheet-shaped molded body, the composite can be manufactured without cutting the boron nitride sintered body and the composite. Further, as compared with the case where the block-shaped boron nitride sintered body and the composite are cut into a sheet shape, the material loss due to processing can be reduced by forming the sheet shape from the stage of the molded body. Therefore, a sheet-like complex can be produced with a high yield.
  • the molded product obtained as described above is heated and fired in, for example, an electric furnace.
  • the heating temperature may be, for example, 1800 ° C. or higher, and may be 1900 ° C. or higher.
  • the heating temperature may be, for example, 2200 ° C. or lower, or 2100 ° C. or lower. If the heating temperature is too low, grain growth tends not to proceed sufficiently.
  • the heating time may be 0.5 hours or more, and may be 1 hour or more, 3 hours or more, 5 hours or more, or 10 hours or more.
  • the heating time may be 40 hours or less, 30 hours or less, or 20 hours or less.
  • the heating time may be, for example, 0.5 to 40 hours, or 1 to 30 hours. If the heating time is too short, grain growth tends not to proceed sufficiently.
  • the heating atmosphere may be, for example, an atmosphere of an inert gas such as nitrogen, helium, or argon.
  • an inert gas such as nitrogen, helium, or argon.
  • a boron nitride sintered body containing boron nitride particles and pores can be obtained. If a thin sheet-shaped molded product is used, a sheet-shaped boron nitride sintered body can be obtained.
  • the fired product containing boron nitride since the fired product containing boron nitride is used, it is possible to prevent the boron nitride particles from being oriented in the direction perpendicular to the thickness direction. Therefore, it is possible to reduce the anisotropy of thermal conductivity and produce a boron nitride sintered body having excellent thermal conductivity along the thickness direction. Further, the pore diameter of the pores contained in the boron nitride sintered body can be reduced as a whole.
  • the range of the orientation index of the boron nitride sintered body is as described above.
  • Boron nitride powder may be used instead of the fired product containing boron nitride.
  • the boron nitride powder for example, one having an average particle size of 15 to 50 ⁇ m can be used.
  • a boron nitride sintered body may be obtained by blending boron nitride powder and the above-mentioned sintering aid and performing the above-mentioned sintering step.
  • the boron nitride sintered body is impregnated with the resin composition.
  • the boron nitride sintered body obtained in the sintering step is in the form of a sheet
  • the boron nitride sintered body can be used as it is without processing.
  • the thickness of the boron nitride sintered body may be 2 mm or less, less than 2 mm, or 1 mm or less.
  • a cutting step of processing the block-shaped boron nitride sintered body into a sheet is performed.
  • the block-shaped boron nitride sintered body may be cut into a sheet having a thickness of, for example, 2 mm or less, and then impregnated with the resin composition.
  • the thickness of the boron nitride sintered body after cutting may be less than 2 mm and may be 1 mm or less.
  • the block-shaped boron nitride sintered body has all sides, for example, when it is a polyhedron. It has a reasonable length and is thicker than the sheet-shaped boron nitride sintered body. That is, the block shape means a shape that can be divided into a plurality of sheet shapes (thin plate shapes) by cutting.
  • the resin composition may be thermosetting, and may be, 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 phosphine-based curing. It may contain at least one curing agent selected from the group consisting of agents and imidazole-based curing agents, and a solvent.
  • the solvent examples include aliphatic alcohols such as ethanol and isopropanol, 2-methoxyethanol, 1-methoxyethanol, 2-ethoxyethanol, 1-ethoxy-2-propanol, 2-butoxyethanol and 2- (2-methoxyethoxy).
  • Ether alcohols such as ethanol, 2- (2-ethoxyethoxy) ethanol, 2- (2-butoxyethoxy) ethanol, glycol ethers such as ethylene glycol monomethyl ether and ethylene glycol monobutyl ether, acetone, methyl ethyl ketone, methyl isobutyl ketone, diisobutyl
  • 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.
  • Resins include epoxy resin, silicone resin, cyanate resin, silicone rubber, acrylic resin, phenol resin, melamine resin, urea resin, bismaleimide resin, unsaturated polyester, fluororesin, polyimide, polyamideimide, polyetherimide, and polybutylene.
  • Telephthalate polyethylene terephthalate, polyphenylene ether, polyphenylene sulfide, total aromatic polyester, polysulfone, liquid crystal polymer, polyether sulfone, polycarbonate, maleimide resin, maleimide-modified resin, ABS (acrylonitrile-butadiene-styrene) resin, AAS (acrylonitrile-acrylic rubber) -Stylus) resin, AES (acrylonitrile, ethylene, propylene, diene rubber-styrene) resin, polyglycolic acid resin, polyphthalamide, polyacetal and the like can be mentioned.
  • One of these may be contained alone, or two or more thereof may be contained in combination.
  • the resin composition may contain an inorganic filler, a silane coupling agent, a defoaming agent, a surface conditioner, a wet dispersant and the like.
  • Impregnation is performed by adhering the resin composition to the boron nitride sintered body.
  • the impregnation method is not particularly limited, but since the boron nitride sintered body has a sufficiently small pore diameter, the resin composition is easily impregnated by the capillary phenomenon. Therefore, a resin composition having a high viscosity can be used, and the resin composition can be applied to the boron nitride sintered body to perform the impregnation step.
  • For coating for example, dip coating, screen printing, transfer printing, offset printing, bar coater, air dispenser, comma coater, gravure coater, letterpress printing, concave printing, gravure printing, stencil printing, soft lithograph, bar coat, applicator, etc.
  • a spin coater, a dip coater, a rubber spatula, a brush, or the like can be used.
  • the boron nitride sintered body Since the boron nitride sintered body has a small pore diameter as a whole, it is easily impregnated with the resin composition due to the capillary phenomenon. Further, if the thickness is 2 mm or less in the form of a sheet, the resin composition can be sufficiently impregnated into the inside. When a sheet-shaped boron nitride sintered body having a thickness of 2 mm or less is impregnated with the resin composition by coating, the viscosity of the resin composition may be 5000 mPa ⁇ s or less, and may be 2000 mPa ⁇ s or less.
  • the viscosity of the resin composition may be 1 mPa ⁇ s or more, and may be 5 mPa ⁇ s or more.
  • the amount of the resin composition applied to the boron nitride sintered body may be 1 to 1.5 times based on the total pore volume of the boron nitride sintered body.
  • a composite having a boron nitride sintered body and a resin filled in its pores can be obtained. It is not necessary that all the pores of the boron nitride sintered body are filled with resin, and some of the pores may not be filled with resin. Boron nitride sintered bodies and complexes may contain both closed and open pores.
  • the impregnation step there may be a curing step of curing the resin filled in the pores.
  • the curing step for example, the composite filled with the resin (resin composition) is taken out from the impregnation device, heated and / or irradiated with light depending on the type of the resin (or the curing agent added as needed). Allows the resin to be cured or semi-cured.
  • the complex thus obtained is, for example, in the form of a sheet and has a thin thickness. Therefore, it is thin and lightweight, and when it is used as a member of an electronic component or the like, it is possible to reduce the size and weight of the electronic component or the like.
  • the pores of the boron nitride sintered body are sufficiently filled with resin, it is also excellent in electrical insulation.
  • the composite in the above-mentioned production method, the composite can be produced without having a step of cutting the boron nitride sintered body and the composite. Therefore, a highly reliable complex can be produced with a high yield.
  • the composite may be used as it is as a heat radiating member, or may be subjected to processing such as polishing to be a heat radiating member.
  • the composite obtained through the cutting step has fine cracks on the cut surface or fine irregularities (striped pattern) generated by cutting.
  • fine cracks and irregularities (striped pattern) on the surface can be sufficiently reduced. Therefore, the composite obtained without undergoing the cutting step can sufficiently improve the electrical insulation property and the thermal conductivity while maintaining a sufficiently high strength. That is, it is excellent in reliability as a member such as an electronic component. Further, when processing such as cutting is performed, material loss occurs. Therefore, the composite having no cut surface can reduce the material loss. Thereby, the yield of the boron nitride sintered body can be improved.
  • the method for producing the composite of the present embodiment includes a nitriding step of calcining boron carbide powder in a nitrogen-pressurized atmosphere to obtain a calcined product containing boron nitride, and a compounding product containing the calcined product and a sintering aid.
  • the nitriding step and the sintering step can be performed in the same manner as in the first embodiment described above.
  • a sheet-shaped boron nitride sintered body not only a sheet-shaped boron nitride sintered body but also a block-shaped boron nitride sintered body can be used.
  • the block-shaped boron nitride sintered body is less likely to be impregnated with the resin composition than the sheet-shaped boron nitride sintered body. Therefore, it is preferable that the impregnation step is performed by immersing the boron nitride sintered body in the resin composition and applying pressure or depressurization conditions in the immersed state.
  • the impregnation step may be performed in an impregnation device provided with a closed container.
  • the pressure in the impregnating device may be increased to be higher than the atmospheric pressure and impregnated under pressurized conditions.
  • the depressurization condition and the pressurization condition may be repeated a plurality of times.
  • 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 solution containing the resin composition may be heated.
  • the viscosity of the solution can be adjusted and the impregnation of the resin composition can be promoted.
  • the viscosity of the solution containing the resin composition at the time of impregnation is preferably 1000 mPa ⁇ s or less, and more preferably 500 mPa ⁇ s or less, from the viewpoint of sufficiently impregnating the pores with the resin composition. As described above, it is necessary to lower the viscosity of the resin composition as compared with the case where the sheet-shaped boron nitride sintered body is impregnated with the resin composition.
  • the boron nitride sintered body can be sufficiently impregnated with the resin composition.
  • the viscosity of the resin composition may be 1 mPa ⁇ s or more, and may be 5 mPa ⁇ s or more.
  • the components of the resin composition are the same as those in the first embodiment.
  • the nitride sintered body is kept immersed in a solution containing the resin composition for a predetermined time.
  • the predetermined time may be, for example, 5 hours or more, or 10 hours or more.
  • the impregnation step may be performed while heating.
  • the resin composition impregnated in the pores of the boron nitride sintered body becomes a resin (cured product or semi-cured product) after curing or semi-curing proceeds or the solvent volatilizes.
  • the impregnation step there may be a curing step of curing the resin filled in the pores.
  • the resin-filled composite is taken out from the impregnation device, and the resin is cured by heating and / or light irradiation depending on the type of resin (or a curing agent added as needed). Or semi-cured.
  • the obtained resin impregnated body is cut using, for example, a wire saw.
  • the wire saw may be, for example, a multi-cut wire saw or the like.
  • a sheet-like composite having a thickness of 2 mm or less can be obtained.
  • the complex thus obtained has a cut surface.
  • the composite obtained by the above-mentioned production method has a porous boron nitride sintered body composed of boron nitride particles and a resin filled in at least a part of the pores of the boron nitride sintered body.
  • the complex may be in the form of a sheet (thin plate shape). The thickness of the complex may be, for example, less than 2 mm.
  • the boron nitride particles that make up the boron nitride sintered body are formed by sintering the primary particles of boron nitride (note that when the primary particles are sintered, the primary particles in the secondary particles are sintered. Including cases.). In the complex, the gaps between the boron nitride particles are filled with resin. Since the complex contains a boron nitride sintered body and a resin, it is excellent in electrical insulation and thermal conductivity.
  • the complex having a thickness of less than 2 mm is thin, it is possible to reduce the size of the electronic component or the like when it is used as a member of the electronic component or the like. Moreover, since it is thin and contains resin, it is possible to reduce the weight.
  • the thickness of the complex may be less than 1 mm and may be less than 0.5 mm.
  • the thickness of the composite may be 0.1 mm or more, and may be 0.2 mm or more.
  • FIG. 1 is a perspective view showing an example of a sheet-like complex.
  • the complex 10 has a thickness t.
  • the thickness t is less than 2 mm.
  • the complex 10 may include a boron nitride sintered body 20 that is uniaxially pressurized and sintered along the thickness direction.
  • the area of the main surface 10a of the complex may be 25 mm 2 or more, 100 mm 2 or more, 800 mm 2 or more, or 1000 mm 2 or more.
  • the thickness t of the complex 10 is small, the resin composition can be smoothly impregnated. Further, since the complex 10 is manufactured using a boron nitride sintered body having a sufficiently small pore diameter, the pores (pores) are sufficiently filled with the resin. Therefore, the voids are sufficiently reduced and the electrical insulation is excellent.
  • the shape of the complex 10 is not limited to the square pillar shape as shown in FIG. 1, and may be, for example, a cylindrical shape or a C-shaped shape in which the main surface 10a is curved.
  • the complex 10 and the boron nitride sintered body 20 do not have to have a cut surface. For example, it may be obtained by sintering a sheet-shaped molded product as shown in FIG. 1 and then impregnating it with a resin composition.
  • Both of the pair of main surfaces 10a and 10b of the complex 10 of FIG. 1 may not be cut surfaces. That is, the side surface of the complex 10 may be a cut surface. In this case as well, it is possible to sufficiently reduce the fine cracks that may occur due to cutting on both of the pair of main surfaces 10a and 10b. Therefore, sufficiently high thermal conductivity can be maintained. Further, the material loss can be reduced as compared with the case where both of the pair of main surfaces 10a and 10b are cut surfaces.
  • the surface of the complex 10 may be shaped by polishing or the like.
  • the orientation index of the boron nitride crystal in the boron nitride sintered body 20 contained in the complex 10 may be 40 or less, 30 or less, 15 or less, and 10 or less. Thereby, the anisotropy of thermal conductivity can be sufficiently reduced. Therefore, the thermal conductivity in the thickness direction of the sheet-shaped boron nitride sintered body can be sufficiently increased.
  • the orientation index of the boron nitride sintered body 20 may be 2.0 or more, 3.0 or more, or 4.0 or more.
  • the orientation index in the present disclosure is an index for quantifying the degree of orientation of boron nitride crystals.
  • the orientation index can be calculated by the peak intensity ratio [I (002) / I (100)] of the (002) plane and the (100) plane of boron nitride measured by an X-ray diffractometer.
  • the average pore diameter of the pores in the boron nitride sintered body 20 may be less than 4.0 ⁇ m. By reducing the size of the pores, the filling rate of the resin can be increased. Therefore, the electrical insulation of the complex 10 can be further improved. From the viewpoint of facilitating the impregnation of the resin composition into the boron nitride sintered body 20, the average pore diameter of the pores may be 0.5 to 3.5 ⁇ m, or 1.0 to 3.0 ⁇ m. good. When the average pore diameter becomes excessive, the penetration of the resin composition due to the capillary phenomenon tends to be difficult to proceed. On the other hand, when the average pore diameter is too small, the porosity of the boron nitride sintered body tends to be small, and the impregnation amount of the resin composition tends to be small.
  • the average pore diameter of the pores is determined based on the pore diameter distribution when the pressure is increased from 0.0042 MPa to 206.8 MPa using a mercury porosimeter.
  • the pore diameter when the cumulative pore volume reaches 50% of the total pore volume is the average pore diameter.
  • the mercury porosimeter one manufactured by Shimadzu Corporation can be used.
  • the porosity of the boron nitride sintered body 20, that is, the volume ratio of the pores in the boron nitride sintered body 20, may be 30 to 65% by volume, 30 to 60% by volume, and 35 to 55% by volume. It may be. If the porosity becomes too large, the strength of the complex 10 tends to decrease. On the other hand, if the porosity becomes too small, the mass tends to be heavy.
  • the bulk density [B (kg / m 3 )] was calculated from the volume and mass of the boron nitride sintered body 20, and the bulk density and the theoretical density of boron nitride [2280 (kg / m 3 )] were used. Therefore, it can be obtained by the following formula (1).
  • Porosity (% by volume) [1- (B / 2280)] x 100 (1)
  • the bulk density B may be 800 to 1500 kg / m 3 , 850 to 1400 kg / m 3 , or 900 to 1300 kg / m 3 . If the bulk density B becomes too large, the mass of the boron nitride sintered body tends to increase. In addition, the filling amount of the resin tends to decrease, and the electrical insulating property of the complex tends to decrease. On the other hand, if the bulk density B becomes too small, the strength of the boron nitride sintered body tends to decrease.
  • the thermal conductivity of the boron nitride sintered body 20 in the thickness direction may be 20 W / (m ⁇ K) or more, 30 W / (m ⁇ K) or more, and 35 W / (m ⁇ K) or more. It may be 40 W / (m ⁇ K) or more.
  • H is the thermal conductivity (W / (m ⁇ K))
  • A is the thermal diffusivity (m 2 / sec)
  • B is the bulk density (kg / m 3 )
  • C is the specific heat capacity. (J / (kg ⁇ K)) is shown.
  • the thermal diffusivity A can be measured by a laser flash method.
  • the bulk density B can be obtained from the volume and mass of the boron nitride sintered body 20.
  • the specific heat capacity C can be measured using a differential scanning calorimeter.
  • the boron nitride sintered body may have the above-mentioned thermal conductivity in the thickness direction.
  • the composite according to one embodiment is a composite of a boron nitride sintered body and a resin, and has the above-mentioned boron nitride sintered body and a resin filled in at least a part of the pores of the boron nitride sintered body. .. Examples of resins are as described above.
  • the resin may contain an epoxy resin from the viewpoint of improving heat resistance and adhesive strength to the circuit.
  • the resin may contain a silicone resin from the viewpoint of improving heat resistance, flexibility, and adhesion to a heat sink or the like.
  • the resin may be a cured product (C stage state) or a semi-cured product (B stage state). Whether or not the resin is in a semi-cured state can be confirmed by, for example, a differential scanning calorimeter.
  • the content of the boron nitride particles in the complex 10 may be 40 to 70% by volume or 45 to 65% by volume based on the total volume of the complex 10.
  • the content of the resin in the complex may be 30 to 60% by volume or 35 to 55% by volume based on the total volume of the complex 10.
  • a complex containing boron nitride particles and a resin in such a proportion can achieve both high electrical insulation and high thermal conductivity at a high level.
  • the content of the resin in the complex 10 may be 10 to 60% by mass, 15 to 60% by mass, or 15 to 50% by mass, based on the total mass of the complex, 20. It may be up to 50% by mass, 25 to 50% by mass, or 25 to 40% by mass.
  • a complex containing a resin in such a ratio can achieve both high insulation and thermal conductivity at a high level.
  • the content of the resin in the complex 10 can be determined by heating the complex 10 to decompose and remove the resin, and calculating the mass of the resin from the mass difference before and after heating.
  • the complex 10 may further contain other components in addition to the boron nitride sintered body and the resin filled in the pores thereof.
  • other components include a curing agent, an inorganic filler, a silane coupling agent, a defoaming agent, a surface conditioner, a wet dispersant and the like.
  • the inorganic filler may contain one or more selected from the group consisting of aluminum oxide, silicon oxide, zinc oxide, silicon nitride, aluminum nitride and aluminum hydroxide. Thereby, the thermal conductivity of the complex can be further improved.
  • the composite 10 of the present embodiment contains the above-mentioned boron nitride sintered body and the resin filled in the pores thereof, it has both excellent thermal conductivity and excellent electrical insulation. Further, since it is thin and lightweight, it is possible to reduce the size and weight of the electronic component when it is used as a member of the electronic component or the like. Since the complex has such characteristics, it can be suitably used as a heat radiating member.
  • the heat radiating member may be composed of the above-mentioned composite, or may be composed of a composite with another member (for example, a metal plate such as aluminum).
  • a boron nitride sintered body may be obtained by hot pressing in which molding and sintering are performed at the same time.
  • Example 1 ⁇ Preparation of Boron Nitride 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 resulting mixture was filled into a graphite crucible. Using an arc furnace, the crucible was heated at 2200 ° C. for 5 hours in an argon atmosphere to obtain massive boron carbide (B 4 C). The obtained mass 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.
  • the carbon content of the obtained boron carbide powder was 19.9% by mass.
  • the amount of carbon was measured with a carbon / sulfur simultaneous analyzer.
  • the prepared boron carbide powder was filled in a crucible made of boron nitride. Then, using a resistance heating furnace, the mixture was heated in a nitrogen gas atmosphere at 2000 ° C. and 0.85 MPa for 10 hours. In this way, a fired 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, 1.9 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 1.2 atomic% of calcium with respect to 100 atomic% of boron. 16 parts by mass of the sintering aid was added to 100 parts by mass of the calcined product and mixed using a Henschel mixer to obtain a powdery compound.
  • a block-shaped (length x width x thickness 49 mm x 25 mm x 57 mm) molded product.
  • 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 block-shaped boron nitride sintered body was obtained. The thickness t of the boron nitride sintered body was 60 mm.
  • H is the thermal conductivity (W / (m ⁇ K))
  • A is the thermal diffusivity (m 2 / sec)
  • B is the bulk density (kg / m 3 )
  • C is the specific heat capacity. (J / (kg ⁇ K)) is shown.
  • a xenon flash analyzer manufactured by NETZSCH, trade name: LFA447NanoFlash
  • the bulk density B was calculated from the volume and mass of the boron nitride sintered body.
  • the results of thermal conductivity H and bulk density B are shown in Table 1.
  • the orientation index [I (002) / I (100)] of the boron nitride sintered body was determined using an X-ray diffractometer (manufactured by Rigaku Co., Ltd., trade name: ULTIMA-IV).
  • the measurement sample (boron nitride sintered body) set in the sample holder of the X-ray diffractometer was irradiated with X-rays to perform baseline correction. Then, the peak intensity ratio of the (002) plane and the (100) plane of boron nitride was calculated. This was defined as the orientation index [I (002) / I (100)].
  • the results are as shown in Table 1.
  • a resin composition containing an epoxy resin (manufactured by Mitsubishi Chemical Corporation, trade name: Epicoat 807) and a curing agent (manufactured by Nippon Synthetic Chemical Industry Co., Ltd., trade name: Acmex H-84B) is subjected to reduced pressure conditions and pressurized conditions.
  • the depressurization condition was 500 Pa ⁇ 30 minutes, and the pressurization condition was 1 MPa ⁇ 30 minutes.
  • the resin was cured by heating at a temperature of 120 ° C. for 120 minutes under atmospheric pressure to obtain a complex.
  • This complex had a thickness (60 mm) equivalent to that of the boron nitride sintered body.
  • the resin content in the complex is as shown in Table 2.
  • the content (mass%) of this resin is the mass ratio of the resin to the entire complex.
  • the resin content was calculated by calculating the mass of the resin from the mass difference between the boron nitride sintered body and the composite, and dividing the mass of this resin by the mass of the composite.
  • the "dielectric breakdown voltage” in the present specification means a value measured by a withstand voltage tester (manufactured by Kikusui Electronics Co., Ltd., device name: TOS-8700) in accordance with JIS C2110-1: 2016.
  • a withstand voltage tester manufactured by Kikusui Electronics Co., Ltd., device name: TOS-8700
  • Example 2 10.7 parts by mass of amorphous boron nitride powder having an oxygen content of 1.7% by mass and an average particle size of 3.4 ⁇ m, and an oxygen content of 0.1% by mass and an average particle size of 16. 7.1 parts by mass of hexagonal boron nitride powder of 0 ⁇ m, 0.9 parts by mass of calcium carbonate (manufactured by Shiraishi Kogyo Co., Ltd., trade name: PC-700), and 1.6 parts by mass of boric acid are mixed with a Henschel mixer. Was mixed to obtain a mixture. Then, 380 parts by mass of water was added to 100 parts by mass of the mixture and pulverized with a ball mill for 5 hours to obtain a water slurry.
  • amorphous boron nitride powder having an oxygen content of 1.7% by mass and an average particle size of 3.4 ⁇ m, and an oxygen content of 0.1% by mass and an average particle size of 16. 7.1 parts by mass of hexagonal boron n
  • Polyvinyl alcohol (manufactured by Nippon Synthetic Chemical Industry Co., Ltd., trade name: Gosenol) was added to this water slurry so that its concentration was 3.0% by mass, and the mixture was heated and stirred at 50 ° C. until it was dissolved. Then, a spheroidizing treatment was performed at a drying temperature of 200 ° C. with a spray dryer to obtain granulated products. A rotary atomizer was used as the spheroidizing device of the spray dryer.
  • 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 2050 ° C. for 10 hours. Then, the boron nitride sintered body was taken out from the boron nitride container. In this way, a block-shaped boron nitride sintered body was obtained.
  • the thickness t of the boron nitride sintered body was 60 mm.
  • Example 1 Each evaluation of the boron nitride sintered body thus obtained was carried out in the same manner as in Example 1. Further, using this boron nitride sintered body, a complex was prepared in the same manner as in Example 1. The thickness of the complex was 60 mm. Then, the dielectric breakdown voltage of the complex was measured in the same manner as in Example 1. The measurement results are as shown in Tables 1 and 2.
  • Example 3 Boron nitride sintered body (thickness: 10 mm) and composite in the same manner as in Example 1 except that the amount of the compound used when producing the molded product was 16.2 g and the thickness of the molded product was 9.5 mm. A body (thickness: 10 mm) was prepared.
  • Example 4 The amount of the compound used when producing the molded product was 3.2 g and the thickness of the molded product was 1.9 mm, and when the composite was produced, boron nitride was sintered using a bar coater under atmospheric pressure. A boron nitride sintered body (thickness: 2.0 mm) and a composite (thickness: 2.0 mm) were produced in the same manner as in Example 1 except that the body was impregnated with the resin composition.
  • Example 5 The amount of the compound used when producing the molded product was 1.6 g, the thickness of the molded product was 0.95 mm, and when the composite was produced, boron nitride was sintered using a bar coater under atmospheric pressure. A sintered body (thickness: 1.0 mm) and a composite (thickness: 1.0 mm) were produced in the same manner as in Example 1 except that the body was impregnated with the resin composition.
  • Example 6 The amount of the compound used when producing the molded product was 0.16 g, the thickness of the molded product was 0.09 mm, and when the composite was produced, boron nitride was sintered using a bar coater under atmospheric pressure. A boron nitride sintered body (thickness: 0.1 mm) and a composite (thickness: 0.1 mm) were prepared in the same manner as in Example 1 except that the body was impregnated with the resin composition.
  • Example 7 The amount of granules used when producing the molded product was 0.15 g, the thickness of the molded product was 0.09 mm, and when the composite was produced, boron nitride was fired using a bar coater under atmospheric pressure.
  • a boron nitride sintered body (thickness: 0.1 mm) and a composite (thickness: 0.1 mm) were produced in the same manner as in Example 2 except that the body was impregnated with the resin composition.
  • Amorphous boron nitride powder (manufactured by Denka Corporation, oxygen content: 1.5%, boron nitride purity: 97.6%, average particle size: 6.0 ⁇ m) is 40.0% by mass and hexagonal boron nitride is placed in a container.
  • the powder (manufactured by Denka Corporation, oxygen content: 0.3%, boron nitride purity: 99.0%, average particle size: 30.0 ⁇ m) was measured so as to be 60.0% by mass.
  • a sintering aid (boric acid and calcium carbonate)
  • an organic binder and water are added and mixed, and then dry granulation is performed to obtain a mixed powder of nitride. It was adjusted.
  • the mixed powder was filled in a cold isotropic pressurization (CIP) device (manufactured by Kobe Steel, Ltd., trade name: ADW800), and the mixed powder was compressed by applying a pressure of 60 MPa to obtain a molded product.
  • CIP cold isotropic pressurization
  • Boron nitride sintered body by holding the obtained molded body at 2000 ° C. for 10 hours and sintering it using a batch type high frequency furnace (manufactured by Fuji Dempa Kogyo Co., Ltd., trade name: FTH-300-1H). was prepared.
  • the firing was carried out by adjusting the inside of the furnace under a nitrogen atmosphere while flowing nitrogen into the furnace in a standard state so that the flow rate was 10 L / min.
  • the obtained boron nitride sintered body has an average pore diameter of 2.5 ⁇ m, a porosity of 58% by volume, an orientation index of 7, a bulk density of 1020 kg / m 3 , and a thermal conductivity of 34 W / (m ⁇ K). Met.
  • the boron nitride sintered body prepared as described above was impregnated with the same thermosetting resin composition as in Example 1 by the following method.
  • a vacuum heating impregnation device manufactured by Kyoshin Engineering Co., Ltd., trade name: G-555AT-R.
  • the inside of the apparatus was degassed for 10 minutes under the conditions of temperature: 100 ° C. and pressure: 15 Pa.
  • the nitride sintered body was immersed in the thermosetting resin composition for 40 minutes while maintaining the same conditions, and the nitride sintered body was impregnated with the thermosetting composition.
  • thermosetting resin composition was impregnated into the nitride sintered body by holding for 120 minutes under the conditions of 130 ° C. and pressure: 3.5 MPa. Then, the nitride sintered body is taken out from the apparatus and heated under the conditions of temperature: 120 ° C. and atmospheric pressure for 8 hours to semi-cure the thermosetting resin composition, thereby filling the boron nitride with a resin.
  • a sintered body (resin impregnated body) was prepared.
  • the content of the semi-cured product in the obtained resin impregnated body was 50% by volume.
  • the size of the resin-impregnated body of the obtained complex was length (length): 50 mm, width (width): 50 mm, and height (thickness): 50 mm.
  • a boron nitride sintered body and a composite which are thin and suitable as members for electronic parts and the like, and a method for producing these are provided. Further, a heat radiating member suitable as a member of an electronic component or the like is provided.

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JP7594335B1 (ja) * 2024-06-07 2024-12-04 アドバンスコンポジット株式会社 ヘキサゴナル窒化ホウ素粒子分散樹脂複合体及びヘキサゴナル窒化ホウ素粒子分散樹脂複合体の製造方法
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