WO2018181606A1 - 伝熱部材及びこれを含む放熱構造体 - Google Patents
伝熱部材及びこれを含む放熱構造体 Download PDFInfo
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- WO2018181606A1 WO2018181606A1 PCT/JP2018/013026 JP2018013026W WO2018181606A1 WO 2018181606 A1 WO2018181606 A1 WO 2018181606A1 JP 2018013026 W JP2018013026 W JP 2018013026W WO 2018181606 A1 WO2018181606 A1 WO 2018181606A1
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- boron nitride
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Definitions
- the present invention provides a heat transfer member having low thermal conductivity anisotropy and excellent reliability, and a heat dissipation structure including the heat transfer member.
- heat-generating electronic components such as power devices, double-sided heat dissipation transistors, thyristors, and CPUs
- heat dissipation measures include (1) increasing the thermal conductivity of the insulating layer of the printed wiring board on which the heat generating electronic components are mounted, and (2) the heat generating electronic components or the printed wiring on which the heat generating electronic components are mounted.
- a heat transfer member obtained by adding and curing a ceramic powder to a silicone resin or an epoxy resin is used.
- hexagonal boron nitride powder having excellent properties as an electrical insulating material such as (1) high thermal conductivity and (2) high insulation is attracting attention.
- boron nitride has a thermal conductivity in the in-plane direction (a-axis direction) of 400 W / (m ⁇ K), which is higher than that of aluminum nitride or silicon nitride, whereas the thermal conductivity in the thickness direction (c-axis direction). Is 2 W / (m ⁇ K), and the thermal conductivity anisotropy derived from the crystal structure and scale shape is large.
- the thermal interface material when the thermal interface material is manufactured, if the in-plane direction of the boron nitride particles (a-axis direction) and the thickness direction of the thermal interface material become perpendicular, the in-plane direction of the boron nitride particles (a-axis direction) The high thermal conductivity of was not able to be fully utilized.
- Patent Document 1 discloses an electronic circuit comprising a ceramic composite comprising a porous ceramic sintered body having a three-dimensional network crystal structure and having open pores, the resin being filled in the open pores. There has been proposed a substrate for an electronic circuit, wherein the porous ceramic sintered body is made of a ceramic material having crystal grains having an average crystal grain size of 10 ⁇ m or less. However, in the method of Patent Document 1, the scaly boron nitride particles are oriented in one direction, and the thermal conductivity anisotropy cannot be reduced.
- Patent Document 2 a ceramic member, which is a sintered body containing at least forsterite and boron nitride as main components and boron nitride is oriented in one direction, a probe holder formed using the ceramic member, and a ceramic member Manufacturing methods have been proposed.
- the degree of orientation of scaly boron nitride O. P. (The Index of Orientation Preferences) was as large as 0.07 or less, and the scaly boron nitride particles were oriented in one direction, and the anisotropy of thermal conductivity could not be reduced.
- the heat transfer members with large thermal conductivity anisotropy of the prior art have restrictions on the arrangement of cooling units and heat transport units, making electronic devices even lighter, thinner and shorter It has become difficult to follow. Therefore, development of a heat transfer member having excellent thermal conductivity and low thermal conductivity anisotropy is strongly expected.
- Patent Document 3 scaly boron nitride particles having a specific calcium content and a graphitization index of boron nitride and having an appropriately controlled average particle size are bonded in a three-dimensional manner with a small degree of orientation of the boron nitride crystal.
- an insulating material A which is a boron nitride-resin composite obtained by combining a resin with a boron nitride sintered body having a small thermal conductivity anisotropy, is disposed as a surface layer
- an insulating material B which is a boron nitride-resin composite obtained by compounding a resin, with respect to a boron nitride sintered body having anisotropy in thermal conductivity and high thermal conductivity
- the present invention is suitably used for heat transfer applications of heat-generating electronic components such as power devices, and particularly used for insulating layers of printed wiring boards, thermal interface materials, power module substrates, and double-sided heat dissipation power modules for automobiles.
- the present invention provides a heat transfer member that is excellent in thermal conductivity and has low thermal conductivity anisotropy and excellent reliability. That is, in the present invention, the following means are adopted.
- a first surface layer comprising insulating material A; A second surface layer comprising insulating material A; An intermediate layer including an insulating material B disposed between the first surface layer and the second surface layer;
- the insulating material A includes a first boron nitride sintered body having a degree of orientation of hexagonal boron nitride primary particles of 0.6 to 1.4, and a first boron nitride sintered body impregnated in the first boron nitride sintered body.
- the insulating material B includes a second boron nitride sintered body in which the degree of orientation of hexagonal boron nitride primary particles is 0.01 to 0.05, and a second boron nitride sintered body impregnated in the second boron nitride sintered body.
- a heat transfer member comprising a thermosetting resin composition.
- the amount of the boron nitride sintered body contained in at least one of the insulating material A and the insulating material B is in a range of 20% by volume to 80% by volume based on the volume of the insulating material. Heat transfer member.
- the heat transfer member is the heat transfer member according to (1) or (2).
- Device heat dissipation structure In the heat dissipating structure of the electric circuit device in which the cooler is disposed in contact with the heat sink via the heat transfer member, the heat transfer member is the heat transfer member according to (1) or (2). Device heat dissipation structure.
- the insulating material A which is a boron nitride-resin composite obtained by combining a resin with a boron nitride sintered body having a small thermal conductivity anisotropy, is disposed as a surface layer, and the thermal conductivity is different.
- Insulating material B which is a boron nitride-resin composite obtained by compounding a resin with a boron nitride sintered body having high thermal conductivity, is not disposed by the conventional technique. In addition, it is possible to obtain a heat transfer member having excellent heat dissipation and low thermal conductivity anisotropy.
- the heat transfer member according to the embodiment of the present invention includes at least two layers of insulating material A and insulating material B sandwiched between the two layers.
- the insulating material A refers to the degree of orientation of primary hexagonal boron nitride particles I.V. O. P.
- a boron nitride sintered body having a (The Index of Orientation Preferences) of 0.01 to 0.05 is impregnated with a thermosetting resin composition.
- the insulating material B is obtained by impregnating a boron nitride sintered body having a degree of orientation of hexagonal boron nitride primary particles of 20 to 100 with a thermosetting resin composition.
- the insulating material A and the insulating material B are preferably flat. The materials and terms used will be described below.
- boron nitride sintered body boron nitride resin composite
- insulating material a material obtained by processing and forming a boron nitride resin composite (preferably in a sheet form) is defined as an “insulating material”.
- the heat radiating plate preferably functions as both an electrode and a heat radiating member, and is preferably made of a metal having good thermal conductivity and electrical conductivity such as a copper alloy or an aluminum alloy.
- the cooler is made of, for example, aluminum, and may be a water-cooled type in which cooling water flows or an air-cooled type having fins.
- O. P. (I100 / I002) par. / (I100 / I002) perp.
- (I100 / I002) par. Is the intensity ratio of the surface measured along the direction parallel to the thickness direction.
- (I100 / I002) perp. Is the intensity ratio of the surface measured from the direction perpendicular to the thickness direction.
- I100 indicates the intensity of the (100) plane X-ray diffraction line
- I002 indicates the intensity of the (002) plane X-ray diffraction line.
- I. O. P. 1, it means that the direction of the boron nitride crystal in the sample is random.
- I. O. P. Is less than 1 means that the (100) plane of the boron nitride crystal, that is, the a-axis of the boron nitride crystal is oriented perpendicular to the thickness direction.
- I. O. P. When the value exceeds 1, it means that the (100) plane of the boron nitride crystal, that is, the a-axis of the boron nitride crystal is oriented parallel to the thickness direction. In general, it is known that the I.O.P.
- thermosetting resin composition I.V. O. P. This is because the thermosetting resin composition is I.V. O. P. This is because the measurement is not affected.
- the amount of the boron nitride sintered body in the boron nitride resin composite is preferably in the range of 20 to 80% by volume (that is, the amount of the thermosetting resin composition is 80 to 20% by volume).
- the insulating material B has a boron nitride sintered body content of 30 to 70% by volume (that is, the thermosetting resin composition is 70-30 volume%), and the insulating material A is 20-30 volume% (the thermosetting resin composition is 80-70 volume) in order to match the anisotropy of thermal conductivity between the insulating material B and the heat sink or cooler. %), Is good. If the amount of the boron nitride sintered body is smaller than 20% by volume, the ratio of the thermosetting resin composition having a low thermal conductivity increases, so that the thermal conductivity decreases.
- the thermosetting resin composition is formed on the surface of the adherend when the adherend such as a metal plate or a metal circuit is bonded to the insulating material by heating and pressing. It becomes difficult for objects to enter, and the tensile shear bond strength and thermal conductivity may decrease.
- the ratio (volume%) of the boron nitride sintered body in the boron nitride resin composite can be determined by measuring the bulk density and porosity of the boron nitride sintered body shown below.
- the boron nitride sintered body of the present invention controls the average major axis and aspect ratio of the boron nitride particles, Since closed pores can be suppressed to 1% or less, they can be ignored. Further, the average pore diameter is not particularly limited, but 0.1 to 3.0 ⁇ m is practical from the viewpoint of impregnation with a thermosetting resin.
- thermosetting resin composition ⁇ Combination of boron nitride sintered body and thermosetting resin composition>
- the boron nitride sintered body and the thermosetting resin composition of the present invention can be combined, for example, by impregnating the boron nitride sintered body with the thermosetting resin composition.
- the impregnation of the thermosetting resin composition can be performed by vacuum impregnation, pressure impregnation at 1 to 300 MPa, or impregnation thereof.
- the pressure during vacuum impregnation is preferably 1000 Pa or less, and more preferably 100 Pa or less.
- thermosetting resin composition In the pressure impregnation, if the pressure is 1 MPa or less, there is a possibility that the thermosetting resin composition cannot be sufficiently impregnated to the inside of the boron nitride sintered body, and if it is 300 MPa or more, the facility becomes large and disadvantageous in terms of cost. In order to easily impregnate the thermosetting resin composition inside the boron nitride sintered body, it is more preferable to reduce the viscosity of the thermosetting resin composition by heating to 100 to 180 ° C. during vacuum impregnation and pressure impregnation. .
- thermosetting resin composition is preferably a single substance or both of a substance having an epoxy group or a cyanate group and a simple substance or a combination of both of a substance having a hydroxyl group or a maleimide group.
- Substances having an epoxy group include bisphenol A type epoxy resins, bisphenol F type epoxy resins, polyfunctional epoxy resins (cresol borac epoxy resins, dicyclopentadiene type epoxy resins, etc.), cyclic aliphatic epoxy resins, glycidyl esters.
- substances having a cyanate group such as type epoxy resins and glycidyl amine type epoxy resins, include 2,2-bis (4-cyanatophenyl) propane, bis (4-cyanato-3,5-dimethylphenyl) methane, 2, Hydroxyl groups such as 2-bis (4-cyanatophenyl) hexafluoropropane, 1,1-bis (4-cyanatophenyl) ethane, 1,3-bis (2- (4-cyanatophenyl) isopropyl) benzene, etc.
- 2,2-bis (4-cyanatophenyl) propane bis (4-cyanato-3,5-dimethylphenyl) methane
- 2, Hydroxyl groups such as 2-bis (4-cyanatophenyl) hexafluoropropane, 1,1-bis (4-cyanatophenyl) ethane, 1,3-bis (2- (4-cyanatophenyl) isopropyl) benzene, etc.
- substances that can be used include phenol novolac resins, 4,4 ′-(dimethylmethyle
- substance having a maleimide group such as bis [2- (2-propenyl) phenol]
- examples of the substance having a maleimide group such as bis [2- (2-propenyl) phenol] include 4,4′-diphenylmethane bismaleimide, m-phenylene bismaleimide, bisphenol A diphenyl ether bismaleimide, and 3,3′-dimethyl- 5,5′-diethyl-4,4′-diphenylmethane bismaleimide, 4-methyl-1,3-phenylene bismaleimide, 1,6′-bismaleimide- (2,2,4-trimethyl) hexane, 4,4 '-Diphenyl ether bismaleimide, 4,4'-diphenylsulfone bismaleimide, 1,3-bis (3-maleimidophenoxy) benzene, 1,3-bis (4-maleimidophen
- thermosetting resin composition a silane coupling agent for improving the adhesion between the boron nitride sintered body and the thermosetting resin composition as appropriate, promoting wettability and leveling improvement and viscosity reduction
- An antifoaming agent, a surface conditioner, and a wetting and dispersing agent for reducing the occurrence of defects during impregnation and curing can be contained.
- the resin contains a single substance or two or more ceramic powders selected from the group consisting of aluminum oxide, silicon oxide, zinc oxide, silicon nitride, aluminum nitride, boron nitride, and aluminum hydroxide.
- the pore surface of the boron nitride sintered body can be subjected to a surface treatment for improving the adhesion between the boron nitride sintered body and the thermosetting resin composition.
- the surface treatment method is carried out by impregnating the pores of the boron nitride sintered body with the silane coupling agent solution before compounding with the thermosetting resin composition, and then removing the solvent by drying or the like. Can do.
- Impregnation of the silane coupling agent solution can be performed by vacuum impregnation, pressure impregnation at 1 to 300 MPa, or impregnation thereof.
- the boron nitride resin composite can also be obtained by semi-curing the thermosetting resin composition combined with the boron nitride sintered body.
- the heating method infrared heating, hot air circulation, oil heating method, hot plate heating method or a combination thereof can be used.
- the semi-curing may be performed as it is using the heating function of the impregnation apparatus after completion of the impregnation, or may be separately performed using a known apparatus such as a hot air circulating conveyor furnace after taking out from the impregnation apparatus.
- the total thickness of the insulating material constituting the heat transfer member is based on the required characteristics of the substrate normally used in the technical field. Although it can be 0.32 mm, it can be changed according to other required characteristics. For example, when insulation at high voltage is not so important and thermal resistance is important, a thin heat transfer member with a total thickness of 0.1 to 0.25 mm can be used, and conversely, insulation at high voltage If the partial discharge characteristics are important, a thick one of 0.35 to 1.0 mm may be used. Further, it is preferable that the insulating material A and the insulating material B are directly bonded without any intervening layer so as not to impair the heat radiation characteristics.
- the surface of the insulating material can be subjected to a surface treatment for improving the adhesion between the insulating material, the heat sink and the cooler.
- the silane coupling agent solution is applied to the surface of the boron nitride resin composite before bonding the heat sink and the cooler to the insulating material, and then the solvent is removed by drying or the like.
- well-known things such as water, alcohol, toluene, can be used for a solvent individually or in combination.
- the functional group which a silane coupling agent has what has reactivity with the functional group which a thermosetting resin has can be selected suitably, for example, an epoxy group, a cyanate group, an amino group, etc. are raised.
- ⁇ Adhesive surface of heat sink and cooler> In order to improve the performance of the insulating material and the heat sink and the cooler, the adhesive surface between the heat sink and the cooler and the insulating layer is subjected to degreasing treatment, sandblasting, etching, various plating treatments, primer treatment such as a silane coupling agent, It is desirable to perform surface treatment such as.
- the surface roughness of the heat sink and the bonding surface of the cooler with the boron nitride resin composite is preferably 0.1 ⁇ m to 15 ⁇ m in terms of 10-point average roughness (Rzjis).
- the surface roughness is 0.1 ⁇ m or less, it is difficult to ensure sufficient adhesion with the insulating material, and if it is 15 ⁇ m or more, defects are likely to occur at the adhesive interface, and the withstand voltage decreases. Adhesion may be reduced.
- the structure of the heat transfer member was fabricated by stacking and assembling the insulating material A, the insulating material B, the insulating material A, and the cooler in order on the heat radiating plate exposed to the outside of the electric circuit device. Thereafter, the semiconductor device was clamped and fixed using a narrow pressure member so that the semiconductor device was sandwiched between the heat sink and the cooler. In this manner, the heat transfer member of this embodiment was mounted on the semiconductor device.
- Example 1> ⁇ Manufacture of insulation material A> ⁇ Creation of sintered boron nitride> Amorphous boron nitride powder (“SP” manufactured by Denka) 17.50% by mass, hexagonal boron nitride powder (“MGP” manufactured by Denka) 7.5% by mass, and calcium carbonate (“PC-700” manufactured by Shiraishi Kogyo Co., Ltd.) After mixing 0.47% by mass using a Henschel mixer, 74.53% by mass of water was added and pulverized with a ball mill for 5 hours to obtain a water slurry.
- SP silicon nitride powder
- MGP hexagonal boron nitride powder
- PC-700 calcium carbonate
- the sintered body is taken out from the boron nitride container and sintered with boron nitride. A ligature was obtained. Thereafter, the boron nitride sintered body was pressurized at 50 MPa using a cold isostatic pressing method (hereinafter referred to as CIP) to increase the density.
- CIP cold isostatic pressing method
- Deaeration was performed in a vacuum of 70 Pa for 20 minutes. Thereafter, the mixture was poured in an amount sufficient to immerse the boron nitride sintered body under vacuum, and impregnated for 30 minutes. Thereafter, the resin was impregnated and cured by pressurizing with nitrogen gas at a pressure of 3 MPa and a temperature of 120 ° C. for 30 minutes to obtain a boron nitride resin composite. Then, it heated at 160 degreeC under atmospheric pressure for 12 hours, and let the resin mixture be a semi-hardened state. Thereafter, it was processed into a sheet having a thickness of 160 ⁇ m using a multi-wire saw (“MWS-32N” manufactured by Takatori) to obtain an insulating material A.
- MFS-32N multi-wire saw
- a mixed powder was prepared using 64.2% by mass and 1.8% by mass of calcium carbonate (“PC-700” manufactured by Shiroishi Kogyo Co., Ltd.) using a known technique. Then, this mixed powder for molding was press-molded into a block shape at 5 MPa.
- the obtained block molded body was sintered at a nitrogen flow rate of 10 L / min in a batch type high frequency furnace to obtain a boron nitride sintered body.
- the obtained boron nitride sintered body was treated with CIP at 50 MPa.
- the resin was impregnated and cured by using nitrogen gas at a pressure of 3 MPa and a temperature of 120 ° C. for 30 minutes to obtain a boron nitride-resin composite. Then, it heated at 160 degreeC under atmospheric pressure for 12 hours, the resin mixture was semi-hardened, and it was set as the boron nitride resin composite. Thereafter, it was processed into a sheet having a thickness of 160 ⁇ m using a multi-wire saw (“MWS-32N” manufactured by Takatori) to obtain an insulating material B.
- MWS-32N multi-wire saw
- Insulating material A, insulating material B, insulating material A, and cooler are laminated in this order on the heat sink, and a vacuum heating press (“MHPC-VF-” is used under the conditions of a pressure of 5 MPa, a heating temperature of 200 ° C. and a heating time of 5 hours.
- MHPC-VF- vacuum heating press
- 350-350-1-45 manufactured by Meiki Seisakusho Co., Ltd. was press-bonded to obtain a laminate.
- each member was adhere
- Example 2 The difference from Example 1 was that the firing temperature at the time of producing the boron nitride sintered body in the production of the insulating material A was set to 2100 ° C.
- Example 3 The difference from Example 1 was that in the production of the insulating material A, the firing temperature at the time of producing the boron nitride sintered body was set to 1800 ° C.
- Example 4 The difference from Example 1 was that in the production of the insulating material B, the CIP at the time of producing the boron nitride sintered body was set to 10 MPa.
- Example 5 The difference from Example 1 was that the CIP at the time of producing the boron nitride sintered body in the production of the insulating material B was set to 100 MPa.
- Example 6> The difference from Example 1 was that in the production of the insulating material A, the treatment by CIP at the time of producing the boron nitride sintered body was not carried out.
- Example 1 The difference from Example 1 was that the insulating material A was not used and only the insulating material B was laminated.
- Example 2 The difference from Example 1 was that the insulating material B was not used and only the insulating material A was laminated.
- Example 3 The difference from Example 1 is that the laminated structure of the insulating material A and the insulating material B is reversed, that is, the insulating material B, the insulating material A, the insulating material B, and the cooler are laminated in this order on the heat sink. It was.
- Example 4 The difference from Example 1 is that the firing temperature at the time of producing the boron nitride sintered body in the production of the insulating material A was 2300 ° C. O. P. Was less than 0.6.
- Example 5 The difference from Example 1 is that in the production of the insulating material A, the raw material composition is 3.30% by mass of amorphous boron nitride powder (“SP” manufactured by Denka), hexagonal boron nitride powder (“MGP” manufactured by Denka) 29. 7% by mass and calcium carbonate (“PC-700” manufactured by Shiroishi Kogyo Co., Ltd.) 0.62% by mass, mixed using a Henschel mixer, added with 66.38% by mass of water, and pulverized with a ball mill for 5 hours Insulation material A.I. O. P. Was higher than 1.4.
- SP amorphous boron nitride powder
- MGP hexagonal boron nitride powder
- PC-700 calcium carbonate
- Example 6 The difference from Example 1 is that the CIP treatment at the time of producing the boron nitride sintered body was performed at 150 MPa in the production of the insulating material B. O. P. Was over 0.05.
- the thermal resistivity in this specification is not just a thermal resistivity of a single insulating material but a thermal resistivity including an interface thermal resistance between an insulating material, a heat sink, and a cooler.
- the measurement sample was a laminate in which a heat sink and a cooler were bonded to both sides of the insulating material, and the transient thermal resistance was measured. Specifically, the time change (time history) until the measured chip temperature converges to a substantially constant value during heating with a certain amount of heat generated on the heater chip was measured.
- “T3Ster” manufactured by Mentor Graphics Corporation is employed as a device for measuring the time change of the chip temperature actual measurement value Ta.
- the etching resist was screen-printed in a circular circuit pattern shape having a diameter of 20 mm on one surface of the laminate, and the etching resist was screen-printed in a solid pattern shape on the other surface.
- the metal plate was etched with a cupric chloride solution to form a circular copper circuit having a diameter of 20 mm on one surface of the laminate.
- electroless Ni—P plating was applied to a thickness of 2 ⁇ m to produce a circuit board for evaluation.
- the circuit board was immersed in insulating oil, an AC voltage was applied between the copper circuit and the copper plate at room temperature, and the dielectric breakdown strength was measured in accordance with JIS C 2110-2: 2016.
- As a measuring instrument “TOS-8700” manufactured by Kikusui Electronics Corporation was used.
- Rate of decrease in dielectric breakdown voltage after 1000 heat cycles ((initial breakdown voltage ⁇ dielectric breakdown voltage after 1000 heat-resistant cycles) ⁇ initial breakdown voltage) ⁇ 100
- the heat transfer member of the present invention is effective for use in general industrial and in-vehicle power modules.
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Abstract
Description
絶縁材Aを含む第一の表面層と、
絶縁材Aを含む第二の表面層と、
前記第一の表面層と前記第二の表面層との間に配される、絶縁材Bを含む中間層と
を含み、
前記絶縁材Aが、六方晶窒化ホウ素一次粒子の配向度が0.6~1.4である第一の窒化ホウ素焼結体と、前記第一の窒化ホウ素焼結体に含浸する第一の熱硬化性樹脂組成物とを含むものであり、
前記絶縁材Bが、六方晶窒化ホウ素一次粒子の配向度が0.01~0.05である第二の窒化ホウ素焼結体と、前記第二の窒化ホウ素焼結体に含浸する第二の熱硬化性樹脂組成物とを含む
ことを特徴とする、伝熱部材。
なおここで配向度は、I.O.P.(The Index of Orientation Preference)を意味し、I.O.P.は下式で算出される。
I.O.P.=(I100/I002)par./(I100/I002)perp.
ここで、(I100/I002)par.は、窒化ホウ素焼結体の厚み方向に平行な方向に沿って測定した面の強度比であり、(I100/I002)perp.は、窒化ホウ素焼結体の厚み方向に垂直な方向に沿って測定した面の強度比であり、I100は(100)面のX線回析線の強度を示し、I002は(002)面のX線回析線の強度を示す。
前記絶縁材A及び前記絶縁材Bのうち少なくとも一方に含まれる窒化ホウ素焼結体の量が、絶縁材の体積を基準として20体積%以上80体積%以下の範囲である、(1)に記載の伝熱部材。
放熱板に、伝熱部材を介して冷却器を接して配置する電気回路装置の放熱構造体において、前記伝熱部材が、(1)または(2)に記載の伝熱部材である、電気回路装置の放熱構造体。
本明細書では、窒化ホウ素一次粒子同士が焼結し3次元的に連続する一体構造をなしたものを「窒化ホウ素焼結体」と定義する。また、窒化ホウ素焼結体と熱硬化性樹脂組成物からなる複合体を「窒化ホウ素樹脂複合体」と定義する。また、窒化ホウ素樹脂複合体を(好ましくはシート状に)加工成形したものを「絶縁材」と定義する。
放熱板は電極及び放熱体の機能を兼ねたものが好ましく、例えば銅合金もしくはアルミ合金等の熱伝導性及び電気伝導性の良い金属で構成されているのが好ましい。
冷却器は、例えばアルミニウム等からなり、内部を冷却水が流れる水冷式やフィンを有する空冷式等のものでもよい。
六方晶窒化ホウ素一次粒子(結晶)の配向度I.O.P.は、層状に形成された窒化ホウ素焼結体の厚み方向に平行な方向に沿って測定した、窒化ホウ素焼結体の面(すなわち、層のfaceに相当する面)のX線回析の(002)回析線と(100)回析線との強度比、および窒化ホウ素焼結体の厚み方向に垂直な方向に沿って測定した、窒化ホウ素焼結体の面(すなわち、層の側面)のX線回析の(002)回析線と(100)回析線との強度比から、下式で算出される。
I.O.P.=(I100/I002)par./(I100/I002)perp.
ここで、(I100/I002)par.は、厚み方向に平行な方向に沿って測定した面の強度比である。(I100/I002)perp.は、厚み方向に垂直な方向から測定した面の強度比である。またI100は(100)面のX線回析線の強度を示し、I002は(002)面のX線回析線の強度を示す。
窒化ホウ素樹脂複合体中の窒化ホウ素焼結体の量は20~80体積%(すなわち熱硬化性樹脂組成物の量は80~20体積%)の範囲内であることが好ましい。より好ましくは熱伝導の異方性を小さくし且つ熱伝導率の両立を達成するために、絶縁材Bは窒化ホウ素焼結体の量が30~70体積%(すなわち熱硬化性樹脂組成物は70~30体積%)、絶縁材Aは絶縁材Bと放熱板または冷却器の間に熱伝導率の異方性を合わせるため20~30体積%(熱硬化性樹脂組成物は80~70体積%)、が良い。窒化ホウ素焼結体の量が20体積%より小さいと熱伝導率の低い熱硬化性樹脂組成物の割合が増えるため、熱伝導率が低下する。窒化ホウ素焼結体の量が80体積%より大きいと、金属板や金属回路等の被着体を絶縁材に加熱加圧により接着する際に、被着体表面の凹凸に熱硬化性樹脂組成物が浸入し難くなり、引っ張りせん断接着強さと熱伝導率が低下する可能性がある。窒化ホウ素樹脂複合体中の窒化ホウ素焼結体の割合(体積%)は、以下に示す窒化ホウ素焼結体のかさ密度と気孔率の測定より求めることができる。
窒化ホウ素焼結体かさ密度(D)=質量/体積 ・・・・・(1)
窒化ホウ素焼結体気孔率=(1-(D/窒化ホウ素の真密度))×100
=熱硬化性樹脂の割合 ・・・・・(2)
窒化ホウ素焼結体の割合=100-熱硬化性樹脂の割合・・・・・(3)
本発明の窒化ホウ素焼結体と熱硬化性樹脂組成物は、例えば窒化ホウ素焼結体に熱硬化性樹脂組成物を含浸させることで、複合化することができる。熱硬化性樹脂組成物の含浸は、真空含浸、1~300MPaでの加圧含浸、又はそれらの組合せの含浸で行うことができる。真空含浸時の圧力は、1000Pa以下が好ましく、100Pa以下が更に好ましい。加圧含浸では、圧力1MPa以下では窒化ホウ素焼結体の内部まで熱硬化性樹脂組成物が十分含浸できない可能性があり、300MPa以上では設備が大規模になるためコスト的に不利である。窒化ホウ素焼結体の内部に熱硬化性樹脂組成物を容易に含浸させるため、真空含浸及び加圧含浸時に100~180℃に加熱し、熱硬化性樹脂組成物の粘度を低下させると更に好ましい。
熱硬化性樹脂組成物としては、エポキシ基、シアネート基を有する物質の単体又は両方と、水酸基、マレイミド基を有する物質の単体又は両方の組み合わせであることが好ましい。エポキシ基を有する物質としては、ビスフェノールA型エポキシ樹脂、ビスフェノールF型エポキシ樹脂、多官能エポキシ樹脂(クレゾールのボラックエポキシ樹脂、ジシクロペンタジエン型エポキシ樹脂等)、環式脂肪族エポキシ樹脂、グリシジルエステル型エポキシ樹脂、グリシジルアミン型エポキシ樹脂等、シアネート基を有する物質としては、2,2-ビス(4-シアナトフェニル)プロパン、ビス(4-シアナト-3,5-ジメチルフェニル)メタン、2,2-ビス(4-シアナトフェニル)ヘキサフルオロプロパン、1,1-ビス(4-シアナトフェニル)エタン、1,3-ビス(2-(4-シアナトフェニル)イソプロピル)ベンゼン等、水酸基を有する物質としては、フェノールノボラック樹脂、4,4'-(ジメチルメチレン)ビス[2-(2-プロペニル)フェノール]等、マレイミド基を有する物質としては、4,4'-ジフェニルメタンビスマレイミド、m-フェニレンビスマレイミド、ビスフェノールAジフェニルエーテルビスマレイミド、3,3'-ジメチル-5,5'-ジエチル-4,4'-ジフェニルメタンビスマレイミド、4-メチル-1,3-フェニレンビスマレイミド、1,6'-ビスマレイミド-(2,2,4-トリメチル)ヘキサン、4,4'-ジフェニルエーテルビスマレイミド、4,4'-ジフェニルスルフォンビスマレイミド、1,3-ビス(3-マレイミドフェノキシ)ベンゼン、1,3-ビス(4-マレイミドフェノキシ)ベンゼン、ビス-(3-エチル-5-メチル-4-マレイミドフェニル)メタン、2,2-ビス[4-(4-マレイミドフェノキシ)フェニル]プロパン等が挙げられる。
窒化ホウ素焼結体の気孔表面には、窒化ホウ素焼結体と熱硬化性樹脂組成物間の密着性を向上させるための表面処理を行うことができる。表面処理方法としては、熱硬化性樹脂組成物との複合化前に、シランカップリング剤溶液を窒化ホウ素焼結体の気孔内に含浸させた後、溶剤を乾燥等で除去することで行うことができる。シランカップリング剤溶液の含浸は、真空含浸、1~300MPaでの加圧含浸、又はそれらの組合せの含浸で行うことができる。また、溶剤は水、アルコール、トルエン等の公知のものを、単体又は組み合わせて用いることができる。シランカップリング剤の有する官能基については、熱硬化性樹脂の有する官能基と反応性を持つものを適宜選択することができ、例えばエポキシ基、シアネート基、アミノ基等が上げられる。
窒化ホウ素焼結体と複合化した熱硬化性樹脂組成物を半硬化状態することでも窒化ホウ素樹脂複合体を得ることができる。加熱方式としては、赤外線加熱、熱風循環、オイル加熱方式、ホットプレート加熱方式又はそれらの組み合わせで行うことができる。半硬化は、含浸終了後に含浸装置の加熱機能を利用してそのまま行っても良いし、含浸装置から取り出した後に、熱風循環式コンベア炉等の公知の装置を用いて別途行っても良い。
伝熱部材を構成する絶縁材の総厚み、すなわち上述したように二層の絶縁材Aとそれに挟まれた絶縁材Bの厚みの合計は、当該技術分野で通常用いられる基板での要求特性から0.32mmとすることもできるが、別の要求特性に応じて変えることもできる。例えば、高電圧での絶縁性があまり重要でなく熱抵抗が重要である場合は、総厚み0.1~0.25mmの薄い伝熱部材を用いることができ、逆に高電圧での絶縁性や部分放電特性が重要である場合には、0.35~1.0mmの厚いものを用いてもよい。また、絶縁材Aと絶縁材Bとは、放熱特性を損わないように、介在層が無く直接接着していることが好ましい。
絶縁材の表面には、絶縁材と放熱板及び冷却器の密着性を向上させるための表面処理を行うことができる。表面処理方法としては、放熱板及び冷却器と絶縁材の接着前に、シランカップリング剤溶液を窒化ホウ素樹脂複合体表面に塗布した後、溶剤を乾燥等で除去することで行うことができる。また、溶剤は水、アルコール、トルエン等の公知のものを、単体又は組み合わせて用いることができる。シランカップリング剤の有する官能基については、熱硬化性樹脂の有する官能基と反応性を持つものを適宜選択することができ、例えばエポキシ基、シアネート基、アミノ基等が上げられる。
絶縁材と放熱板及び冷却器の性能を向上させるために、放熱板及び冷却器と絶縁層との接着面に、脱脂処理、サンドブラスト、エッチング、各種メッキ処理、シランカップリング剤等のプライマー処理、等の表面処理を行うことが望ましい。また、放熱板及び冷却器の窒化ホウ素樹脂複合体との接着面の表面粗さは、十点平均粗さ(Rzjis)で0.1μm~15μmが好ましい。表面粗さが0.1μm以下であると絶縁材と十分な密着性を確保することが困難であり、また15μm以上であると接着界面で欠陥が発生し易くなり、耐電圧が低下したり、密着性が低下する可能性がある。
<絶縁材Aの製造>
<窒化ホウ素焼結体の作成>
アモルファス窒化ホウ素粉末(「SP」デンカ社製)17.50質量%、六方晶窒化ホウ素粉末(「MGP」デンカ社製)7.5質量%及び炭酸カルシウム(「PC-700」白石工業社製)0.47質量%をヘンシェルミキサーを用いて混合した後、水74.53質量%を添加してボールミルで5時間粉砕し、水スラリーを得た。さらに、得られた水スラリーの総質量に対して、ポリビニルアルコール樹脂(「ゴーセノール」日本合成化学社製)を0.5質量%となるように添加し、溶解するまで50℃で加熱撹拌した後、噴霧乾燥機にて乾燥温度230℃で球状化処理を行った。なお、噴霧乾燥機の球状化装置としては、回転式アトマイザーを使用した。得られた処理物を窒化ホウ素製容器に充填し、バッチ式高周波炉にて窒素流量5L/min、2000℃で常圧焼結させた後、窒化ホウ素容器から焼結体を取り出して窒化ホウ素焼結体を得た。その後、冷間等方圧加圧法(以下CIPと記す。)を用いて窒化ホウ素焼結体を50MPaで加圧し、高密度化を行った。
得られた窒化ホウ素焼結体に樹脂含浸を行った。窒化ホウ素焼結体と、ビスフェノールF型エポキシ樹脂(「JER807」三菱化学社製)12.10質量%、ノボラック型シアネート樹脂(「PT-30」ロンザ社製、日本合成化工社販売)72.00質量%、フェノールノボラック樹脂「TD-2131」(DIC社製)7.9質量%、4,4'-ジフェニルメタンビスマレイミド樹脂「BMI」(ケイ・アイ化成社製)8.0質量%の混合物を圧力70Paの真空中で20分間脱気した。その後に真空下で当該混合物を窒化ホウ素焼結体が漬かる程度の量注ぎ込み、30分間含浸した。その後、窒素ガスを用いて圧力3MPa、温度120℃で30分間加圧して樹脂を含浸・硬化させ、窒化ホウ素樹脂複合体を得た。その後、大気圧下、160℃で12時間加熱し、樹脂混合物を半硬化状態とした。その後、マルチワイヤーソー(「MWS-32N」タカトリ社製)を用いて、160μmの厚さのシート状に加工し、絶縁材Aを得た。
<窒化ホウ素焼結体の作成>
酸素含有量1.5%、窒化ホウ素純度97.6%、及びアモルファス窒化ホウ素粉末34.0質量%、酸素含有量0.3%、窒化ホウ素純度99.0%、である六方晶窒化ホウ素粉末64.2質量%及び炭酸カルシウム(「PC-700」白石工業社製)1.8質量%を、公知の技術を用いて混合粉を作製した。そして、この成形用の混合粉末を用いて、5MPaでブロック状にプレス成形した。得られたブロック成形体をバッチ式高周波炉にて窒素流量10L/minで焼結させることで窒化ホウ素焼結体を得た。得られた窒化ホウ素焼結体をCIPにより50MPaで処理を行った。
得られた窒化ホウ素焼結体へ樹脂含浸を行った。窒化ホウ素焼結体ビスフェノールF型エポキシ樹脂(「JER807」三菱化学社製)12.10質量%、ノボラック型シアネート樹脂(「PT-30」ロンザ社製、日本合成化工社販売)72.00質量%、フェノールノボラック樹脂「TD-2131」(DIC社製)7.9質量%、4,4'-ジフェニルメタンビスマレイミド樹脂「BMI」(ケイ・アイ化成社製)8.0質量%を有する樹脂混合物を圧力70Paの真空中で20分間脱気した後、真空下で当該樹脂混合物を窒化ホウ素焼結体が漬かる程度の量注ぎ込み、30分間含浸した。その後、窒素ガスを用いて圧力3MPa、温度120℃で30分間加圧して樹脂を含浸・硬化させ、窒化ホウ素-樹脂複合体を得た。その後、大気圧下、160℃で、12時間で加熱し、樹脂混合物を半硬化させ、窒化ホウ素樹脂複合体とした。その後、マルチワイヤーソー(「MWS-32N」タカトリ社製)を用いて、160μmの厚さのシート状に加工し、絶縁材Bを得た。
放熱板上に、絶縁材A、絶縁材B、絶縁材A、冷却器の順に積層し、圧力5MPa、加熱温度200℃、加熱時間5時間の条件で、真空加熱プレス機(「MHPC-VF-350-350-1-45」名機製作所社製)を用いてプレス接着し積層体を得た。尚各部材間は絶縁材から溶融する樹脂で接着した。
実施例1と異なる点は絶縁材Aの製造において窒化ホウ素焼結体作製時の焼成温度を2100℃とした点であった。
実施例1と異なる点は絶縁材Aの製造において窒化ホウ素焼結体作製時の焼成温度を1800℃とした点であった。
実施例1と異なる点は絶縁材Bの製造において窒化ホウ素焼結体作製時のCIPを10MPaとした点であった。
実施例1と異なる点は絶縁材Bの製造において窒化ホウ素焼結体作製時のCIPを100MPaとした点であった。
実施例1と異なる点は絶縁材Aの製造において窒化ホウ素焼結体作製時のCIPによる処理を未実施とした点であった。
実施例1と異なる点は絶縁材Aを用いず、絶縁材Bのみを積層した点であった。
実施例1と異なる点は絶縁材Bを用いず、絶縁材Aのみを積層した点であった。
実施例1と異なる点は絶縁材Aと絶縁材Bの積層構成を逆にしたこと、すなわち放熱板上に絶縁材B、絶縁材A、絶縁材B、冷却器の順番で積層した点であった。
実施例1と異なる点は絶縁材Aの製造において窒化ホウ素焼結体作製時の焼成温度を2300℃としたために、絶縁材AのI.O.P.が0.6を下回った点であった。
実施例1と異なる点は、絶縁材Aの製造において原料配合をアモルファス窒化ホウ素粉末(「SP」デンカ社製)3.30質量%、六方晶窒化ホウ素粉末(「MGP」デンカ社製)29.7質量%及び炭酸カルシウム(「PC-700」白石工業社製)を0.62質量%、ヘンシェルミキサーを用いて混合した後、水66.38質量%を添加してボールミルで5時間粉砕したために、絶縁材AのI.O.P.が1.4を上回った点であった。
実施例1と異なる点は絶縁材Bの製造において窒化ホウ素焼結体作製時のCIP処理を150MPaで行ったために、絶縁材BのI.O.P.が0.05を上回った点であった。
本明細書における熱抵抗率は、単なる絶縁材単体の熱抵抗率ではなく、絶縁材と放熱板、冷却器との界面熱抵抗も含んだ熱抵抗率である。測定試料は絶縁材の両面に放熱板と冷却器を接着した積層体を用い、過渡熱抵抗を測定した。具体的には、ヒータ用チップに一定の発熱量を与えた加熱時における、チップ温度実測値がほぼ一定の値に収束するまでの時間変化(時刻歴)を測定した。本実施形態では、チップ温度実測値Taの時間変化を測定する装置として、Mentor Graphics Corporation製の「T3Ster」を採用した。
積層体の一方の面にエッチングレジストを直径20mmの円形の回路パターン形状にスクリーン印刷し、また他方の面にエッチングレジストをベタパターン形状にスクリーン印刷した。エッチングレジストを紫外線硬化した後に、金属板を塩化第二銅液でエッチングし、積層体の一方の面に直径20mmの円形の銅回路を形成した。次いで、レジストをアルカリ溶液にて剥離した後、無電解Ni-Pメッキを2μmの厚さで施して評価用の回路基板を製造した。回路基板を絶縁油中に浸漬し、室温で交流電圧とを銅回路と銅板間に印加させ、絶縁破壊強さをJIS C 2110-2:2016に準拠して測定した。測定器には、菊水電子工業社製の「TOS-8700」を用いた。
エッチング後の窒化ホウ素樹脂複合体回路基板の絶縁破壊電圧をJIS C 2141:1992に準拠して測定した。次に、窒化ホウ素樹脂複合体回路基板を、-40℃にて30分、125℃にて30分を1サイクルとする耐熱サイクル試験にて1000サイクル繰り返し試験を行った後、外観及び超音波探傷装置にて金属回路の接着状態を確認した。接着状態は超音波探傷装置にて耐熱サイクル試験前後での接合面積から比較した。超音波探傷像において剥離は接合部内の黒色部で示されることから、この黒色部面積が耐熱サイクル試験前後で大きくなる場合を剥離と定義した。さらに、絶縁破壊電圧を測定し、以下の式で示す熱サイクル1000回後の絶縁破壊電圧の低下率を算出した。低下率が20%以下であるものを合格とした。
熱サイクル1000回後の絶縁破壊電圧の低下率(%)=((初期の絶縁破壊電圧-耐熱サイクル1000回後の絶縁破壊電圧)÷初期の絶縁破壊電圧)×100
2 窒化ホウ素焼結体(I.O.P.=0.6~1.4)に樹脂を含浸して成る絶縁材A
3 窒化ホウ素焼結体(I.O.P.=0.01~0.05)に樹脂を含浸して成る絶縁材B
4 冷却器
Claims (3)
- 絶縁材Aを含む第一の表面層と、
絶縁材Aを含む第二の表面層と、
前記第一の表面層と前記第二の表面層との間に配される、絶縁材Bを含む中間層と
を含み、
前記絶縁材Aが、六方晶窒化ホウ素一次粒子の配向度が0.6~1.4である第一の窒化ホウ素焼結体と、前記第一の窒化ホウ素焼結体に含浸する第一の熱硬化性樹脂組成物とを含むものであり、
前記絶縁材Bが、六方晶窒化ホウ素一次粒子の配向度が0.01~0.05である第二の窒化ホウ素焼結体と、前記第二の窒化ホウ素焼結体に含浸する第二の熱硬化性樹脂組成物とを含む
ことを特徴とする、伝熱部材。
なおここで配向度は、I.O.P.(The Index of Orientation Preference)を意味し、I.O.P.は下式で算出される。
I.O.P.=(I100/I002)par./(I100/I002)perp.
ここで、(I100/I002)par.は、窒化ホウ素焼結体の厚み方向に平行な方向に沿って測定した面の強度比であり、(I100/I002)perp.は、窒化ホウ素焼結体の厚み方向に垂直な方向に沿って測定した面の強度比であり、I100は(100)面のX線回析線の強度を示し、I002は(002)面のX線回析線の強度を示す。 - 前記絶縁材A及び前記絶縁材Bのうち少なくとも一方に含まれる窒化ホウ素焼結体の量が、絶縁材の体積を基準として20体積%以上80体積%以下の範囲である、請求項1に記載の伝熱部材。
- 放熱板に、伝熱部材を介して冷却器を接して配置する電気回路装置の放熱構造体において、前記伝熱部材が、請求項1または2に記載の伝熱部材である、電気回路装置の放熱構造体。
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WO2019172345A1 (ja) * | 2018-03-07 | 2019-09-12 | デンカ株式会社 | セラミックス樹脂複合体と金属板の仮接着体、その製造方法、当該仮接着体を含んだ輸送体、およびその輸送方法 |
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Also Published As
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EP3605602B1 (en) | 2022-01-12 |
US20200031723A1 (en) | 2020-01-30 |
CN110168719B (zh) | 2023-09-01 |
EP3605602A4 (en) | 2020-04-22 |
CN110168719A (zh) | 2019-08-23 |
JP7053579B2 (ja) | 2022-04-12 |
KR20190132395A (ko) | 2019-11-27 |
US11034623B2 (en) | 2021-06-15 |
EP3605602A1 (en) | 2020-02-05 |
JPWO2018181606A1 (ja) | 2020-02-13 |
KR102438540B1 (ko) | 2022-08-30 |
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