WO2022163646A1 - 窒化ホウ素焼結体シートの製造方法、及び焼結体シート - Google Patents

窒化ホウ素焼結体シートの製造方法、及び焼結体シート Download PDF

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WO2022163646A1
WO2022163646A1 PCT/JP2022/002676 JP2022002676W WO2022163646A1 WO 2022163646 A1 WO2022163646 A1 WO 2022163646A1 JP 2022002676 W JP2022002676 W JP 2022002676W WO 2022163646 A1 WO2022163646 A1 WO 2022163646A1
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sheet
sintered body
boron nitride
sintered
sintering aid
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French (fr)
Japanese (ja)
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敦也 鈴木
厚樹 五十嵐
賢久 上島
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Denka Co Ltd
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Denka Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
    • C01B21/064—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with boron
    • 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
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
    • C04B35/583—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on boron nitride
    • 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
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/64—Burning or sintering processes

Definitions

  • Components such as power devices, transistors, thyristors, and CPUs are required to efficiently dissipate the heat generated during use.
  • Boron nitride a type of ceramic, has excellent lubricity, thermal conductivity, and insulation. For this reason, the use of boron nitride and materials obtained by compounding it with other materials as insulating layers and thermal interface materials as described above has been studied.
  • Patent Document 1 a boron nitride molded body is compounded with a resin, and the degree of orientation and graphitization index of boron nitride are set in a predetermined range to achieve excellent thermal conductivity while reducing the anisotropy of thermal conductivity. A technique to do so has been proposed.
  • One aspect of the present disclosure is a step of firing a laminate of green sheets containing boron carbonitride and a sintering aid in a closed space formed by partitioning a portion of the firing furnace to obtain a fired body. and obtaining a sintered sheet from the sintered body by opening the closed section and subjecting the sintered body to heat treatment at 1800 to 2020°C.
  • the green sheet is fired in a closed space formed by partitioning a part of the firing furnace, so that the sintering aid is sufficiently present.
  • a sheet-like sintered body of boron can be formed, and in such a situation needles of hexagonal boron nitride are formed in the intergranular spaces formed by agglomerated particles composed of primary particles of hexagonal boron nitride. Crystals can be grown. The acicular crystals serve as heat transfer paths between the aggregated particles, and can improve the thermal conductivity of the sintered body sheet.
  • the sintering atmosphere is released and heat treatment is performed to volatilize and remove the glass phase and the like derived from the sintering aid formed between the sheet-shaped sintered bodies.
  • heat treatment is performed to volatilize and remove the glass phase and the like derived from the sintering aid formed between the sheet-shaped sintered bodies.
  • the content of the sintering aid may be 6.0% by mass or more based on the total amount of the green sheet.
  • the method for manufacturing the boron nitride sintered body sheet may further include a step of cooling the fired body to 25°C.
  • Boron nitride sintered bodies tend to shrink when heated and expand when cooled. For this reason, before the fired body is heat-treated, the sintered body is once cooled to expand the sintered body, and then heat-treated to shrink the sintered body again, thereby adding strain to the glass phase. By promoting the volatilization of the phase, the separation between the sintered body sheets can be facilitated, and the yield can be further improved.
  • the volume of the closed space is A [unit: L]
  • the total amount of the sintering aid put into the closed space [unit: kg] is B.
  • the B/A value may be 0.040 kg/L or more.
  • One aspect of the present disclosure provides a boron nitride sintered sheet having a maximum height roughness Rz of 12 to 18 ⁇ m on at least one main surface.
  • the sintered sheet has a surface such that the maximum height roughness Rz of at least one main surface is within a predetermined range, and thus has excellent thermal conductivity.
  • the aggregated particles are pushed up as they grow.
  • micrometer-scale unevenness may occur on the surface of the sintered body sheet.
  • the growth of the needle-like crystals progresses to such an extent that the maximum height roughness Rz on the main surface of the sintered sheet is within a predetermined range, so that the sintered sheet exhibits excellent thermal conductivity. obtain.
  • the sintered sheet may have a thickness of less than 2 mm.
  • FIG. 1 is an SEM photograph showing a part of a cross section of a hexagonal boron nitride sintered body.
  • each component in the composition means the total amount of the multiple substances present in the composition unless otherwise specified when there are multiple substances corresponding to each component in the composition.
  • the “steps” used herein may be independent steps or consecutive steps.
  • One embodiment of the method for producing a hexagonal boron nitride sintered body includes a step of firing a raw material powder containing boron carbide in an atmosphere containing nitrogen to obtain boron carbonitride (nitriding step); a step of firing a laminate of green sheets containing a binding agent in a closed space formed by partitioning a part of a firing furnace to obtain a fired body (firing step); a step of obtaining a sintered body sheet from the sintered body (heat treatment step) by heat-treating at 1800 to 2020°C.
  • a raw material powder containing boron carbide (B 4 C) can be prepared, for example, by the following procedure. After mixing boric acid and acetylene black, the mixture is heated in an inert gas atmosphere at 1800 to 2400° C. for 1 to 10 hours to obtain lumps containing boron carbide. The mass can be prepared by grinding, washing, removing impurities, and drying.
  • nitriding step powder containing boron carbide is fired in an atmosphere containing nitrogen to obtain a fired product containing boron carbonitride (B 4 CN 4 ).
  • the firing temperature in the nitriding step may be 1800° C. or higher, or 1900° C. or higher. Also, the firing temperature may be 2400° C. or lower, or 2200° C. or lower. The firing temperature may be, for example, 1800-2400.degree.
  • the lower limit of the nitrogen partial pressure in the nitriding step may be 0.6 MPa or higher, or 0.7 MPa or higher.
  • the upper limit of the nitrogen partial pressure may be 1.0 MPa or less, or 0.9 MPa or less.
  • the nitrogen partial pressure may be, for example, 0.6-1.0 MPa. If the nitrogen partial pressure is too low, the 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 rise.
  • the pressure in this specification is an absolute pressure.
  • the nitrogen gas concentration of the atmosphere containing nitrogen in the nitriding step may be 95.0% by volume or more, or 99.9% by volume or more.
  • the above nitrogen gas concentrations are volume-based concentrations at standard conditions.
  • the firing time in the nitriding step is not particularly limited as long as the boron carbide is sufficiently nitrided, and may be, for example, 6 to 30 hours or 8 to 20 hours.
  • Boron carbonitride prepared in the nitriding process can be obtained as a lump. Therefore, boron carbonitride may be pulverized and used as a powder. Crushing may be performed using a pulverizer. Pulverizers include roller mills, jet mills, hammer mills, pin mills, rotary mills, vibration mills, planetary mills, attritors, bead mills, ball mills, and the like. The pulverization conditions can be adjusted so that the obtained boron carbonitride has a desired average particle size, specific surface area, and the like. Crushing may be performed, for example, by performing treatment for about 20 hours using a ball mill.
  • the lower limit of the average particle size of boron carbonitride may be, for example, 15 ⁇ m or more, 20 ⁇ m or more, or 25 ⁇ m or more.
  • the upper limit of the average grain size of boron carbonitride may be, for example, 50 ⁇ m or less, 40 ⁇ m or less, or 35 ⁇ m or less.
  • the average particle size of the boron carbonitride may be adjusted within the ranges described above, and may be, for example, 15-50 ⁇ m, 15-35 ⁇ m, or 20-35 ⁇ m.
  • the average particle size of boron carbonitride in the present specification is a value obtained by measuring the boron carbonitride powder without homogenizer treatment, and is the average particle size including aggregated particles.
  • the above average particle diameter shall be measured using a particle size distribution analyzer in accordance with ISO 13320:2009.
  • the average particle size obtained by the above measurement is the average particle size by volume statistical value, and the average particle size is the median value (d50).
  • water is used as a solvent for dispersing the aggregates, and hexametaphosphoric acid is used as a dispersant.
  • the lower limit of the specific surface area of boron carbonitride may be, for example, 10 m 2 /g or more, 12 m 2 /g or more, or 14 m 2 /g or more.
  • the upper limit of the specific surface area of boron carbonitride may be, for example, 30 m 2 /g or less, 25 m 2 /g or less, or 20 m 2 /g or less.
  • the specific surface area of boron carbonitride may be adjusted within the above range, and may be, for example, 10-30 m 2 /g, or 12-20 m 2 /g.
  • the specific surface area of the hexagonal boron nitride powder shall be measured using a measuring device in accordance with JIS Z 8803:2013.
  • the specific surface area is a value calculated by applying the BET single-point method using nitrogen gas.
  • Boron carbonitride may be prepared separately, or may be commercially available containing aggregated particles of boron nitride. In this case, the nitriding step may be omitted. Boron carbonitride may have, for example, an average particle size of 15 to 35 ⁇ m and a specific surface area of 10 to 30 m 2 /g.
  • the sheet (also referred to as a green sheet) containing the boron carbonitride and the sintering aid used in the firing step is a sheet formed by mixing the boron carbonitride and the sintering aid. good.
  • a binder may be added to facilitate the formation of the sheet.
  • the boron carbonitride and the sintering aid may be blended in advance, for example, using a mixer such as a Henschel mixer.
  • a sintering aid is a component that promotes the reaction that produces boron nitride from boron carbonitride and the densification of boron nitride.
  • the sintering aid may contain a boron compound having oxygen as a constituent element and a calcium compound.
  • Boron compounds include, for example, boric acid, boron oxide, borax, and diboron trioxide.
  • Examples of calcium compounds include calcium carbonate and calcium oxide.
  • the sintering aid may contain components other than the boron compound and calcium carbonate. Such ingredients include, for example, lithium carbonate and alkali metal carbonates such as sodium carbonate.
  • the content of the sintering aid may be 6.0% by mass or more based on the total amount of the sheet (the total amount of the green sheet). It may be 0% by mass or more, 12.5% by mass or more, or 15.0% by mass or more.
  • the upper limit of the content of the sintering aid may be, for example, 35.0% by mass or less, or 30.0% by mass or less based on the total amount of the sheet.
  • the content of the sintering aid may be adjusted within the above range, and may be, for example, 6.0 to 35.0% by mass based on the total amount of the sheet (the total amount of the green sheet).
  • the binder can be used to form a powder containing boron carbonitride and a sintering aid into a sheet.
  • the binder may be an organic polymer or the like that can be removed by heat treatment in a firing step or the like.
  • an acrylic resin or the like can be used as the binder.
  • the binder content is, for example, 0.1 to 8% by mass, 0.2 to 6% by mass, 0.3 to 4% by mass, or 0.4 to 2% by mass based on the total amount of the green sheet. you can
  • a closed space is formed by dividing a part of the firing furnace. Firing with The closed space may be any space that does not allow the sintering aid to easily move from the space where the sheet exists to the outside space when the sintering aid volatilizes due to heating. may
  • the closed space only needs to be able to isolate the external environment from the internal environment, and may be, for example, a container having a lid or a door. In this case, for example, the entire container may be placed in a firing furnace and heated.
  • the firing process may be performed by adjusting the amount of sintering aid in the closed space.
  • the volume of the closed space is A [unit: L]
  • the total amount of the sintering aid introduced into the closed space [unit: kg] is B/A
  • the amount of the sintering aid in the closed space may be adjusted so that the value of is 0.040 kg/L or more.
  • the sintering aid charged into the closed space is not limited to that mixed with the green sheet. In other words, if necessary, a sintering aid is separately injected into the closed space to increase the vapor pressure of the sintering aid generated in the space, thereby increasing the sintering aid when the green sheet is heated.
  • the above B/A can be adjusted, for example, by adding a sintering aid to the inside of the closed space. Although it depends on the size of , for example, it may be adjusted by stacking about 8 to 12 sheets.
  • the lower limit of the B/A value is, for example, 0.045 kg/L or more, 0.050 kg/L or more, 0.055 kg/L or more, 0.060 kg/L or more, or 0.065 kg/L or more. you can When the lower limit value of B/A is within the above range, the growth of needle-like crystals of hexagonal boron nitride can be promoted, and a sintered body having excellent thermal conductivity can be prepared.
  • the upper limit of the B/A value may be, for example, 0.20 kg/L or less, 0.15 kg/L or less, 0.10 kg/L or less, or 0.90 kg/L or less. By setting the upper limit of B/A within the above range, it is possible to suppress an increase in manufacturing cost.
  • the above B/A may be adjusted within the above range, and may be, for example, 0.045-0.25 kg/L.
  • the pressure in the firing step may be, for example, heating in an atmosphere of normal pressure (atmospheric pressure: 101 kPa), heating in an atmosphere of 50 kPa or less, or heating at a pressure exceeding atmospheric pressure. good too. When pressurized, it may be, for example, 0.5 MPa or less, 0.4 MPa or less, or 0.3 MPa or less.
  • the heat treatment step is a step of opening the closed space and heat-treating the object to be heat-treated at 1800-2020°C.
  • the amount of the glass phase derived from the sintering aid formed between the sintered sheets can be reduced, and the yield in the method for manufacturing the sintered sheets can be improved.
  • the firing process is performed by storing the green sheet in a container with a lid and heat-treating it in a firing furnace
  • the closed space can be opened by opening the lid of the container.
  • the vapor pressure of the sintering aid in the atmosphere surrounding the sintered body is relatively lowered, and the glass phase derived from the sintering aid, etc. is easily removed when heated. Become.
  • the lower limit of the heating temperature in the heat treatment step may be, for example, 1850°C or higher, or 1900°C or higher. By setting the lower limit of the heating temperature within the above range, the glass phase derived from the sintering aid can be more sufficiently reduced.
  • the upper limit of the heating temperature in the heat treatment step may be, for example, 2100° C. or lower, or 2050° C. or lower. By setting the upper limit of the heating temperature within the above range, excessive grain growth of hexagonal boron nitride in the vicinity of the main surface of the sintered body sheet can be suppressed, and the adhesion of the sintered body sheet can be adjusted. can be done.
  • the heating time in the heat treatment step may be 1 hour or longer, 1.5 hours or longer, or 2 hours or longer.
  • the heating time in the heat treatment step may be 10 hours or less, 8 hours or less, or 7 hours or less.
  • the method for manufacturing the above-described boron nitride sintered sheet may have other steps.
  • the above-described method for producing a boron nitride sintered body sheet may further include, for example, the step of cooling the fired body to 25°C.
  • the sintered sheets are loosely bonded after the heat treatment process, the sintered sheets are separated from each other to separate the individual sintered sheets. It may have a stripping step to obtain.
  • An embodiment of the sintered sheet is a boron nitride sintered sheet having a maximum height roughness Rz of 12 to 18 ⁇ m on at least one main surface. At least one of the pair of main surfaces of the sintered body sheet is preferably not a cut surface, and both sides are preferably not a cut surface. At least one of the pair of main surfaces of the sintered body sheet is preferably not a polished surface, and neither of the two surfaces is preferably a polished surface.
  • the sintered sheet can be produced, for example, by the method for producing a boron nitride sintered sheet described above.
  • the sintered sheet may contain a plurality of aggregated particles composed of agglomerated primary particles of boron nitride and a plurality of acicular crystals composed of boron nitride.
  • FIG. 1 is an SEM photograph showing an example of a sintered body sheet, showing a part of a cross section of a hexagonal boron nitride sintered body.
  • the sintered sheet is composed of a plurality of aggregated particles 12 and a plurality of acicular crystals 22 . It can be confirmed from FIG. 1 that needle-like crystals 22 of hexagonal boron nitride are formed in the gaps between the aggregated particles 12 .
  • the plurality of needle-like crystals 22 are in direct or indirect contact with the two or more aggregated particles 12 .
  • the thermal conductivity of the sintered body sheet can be improved.
  • the maximum height roughness Rz on the main surface of the boron nitride sintered body sheet may be, for example, 14 to 18 ⁇ m, or 15 to 18 ⁇ m. It is more preferable that both the maximum height roughnesses Rz on both main surfaces of the sintered body sheet are within the above range.
  • the thermal conductivity can be improved, and since it has an appropriate roughness, adhesion with the adherend can improve sexuality.
  • the arithmetic mean roughness Ra on the main surface of the boron nitride sintered body sheet may be, for example, 1.5 to 3.0 ⁇ m, or 1.0 to 2.8 ⁇ m. More preferably, the arithmetic mean roughness Ra on both main surfaces of the sintered body sheet is within the above range.
  • the arithmetic mean roughness of the principal surface of the boron nitride sintered body sheet is within the above range, the uniformity within the principal surface is more excellent, and the reliability after adhesion to the adherend can be improved.
  • the maximum height roughness Rz and arithmetic mean roughness Ra of the boron nitride sintered body sheet are determined according to JIS B 0601: 2013 "Product Geometric Characteristics Specifications (GPS) - Surface Texture: Contour Method - Terms, Definitions and Surface Texture Parameters are the parameters described in .
  • the thickness of the sintered sheet may be, for example, less than 2 mm or less than 1.6 mm. With a sintered sheet having such a thickness, for example, it becomes easier to fill the pores of the sintered sheet with a resin, and a composite sheet having an excellent resin filling rate can be more easily prepared. be able to. From the viewpoint of ease of manufacturing the sintered sheet, the thickness of the sintered sheet may be, for example, 0.1 mm or more, or 0.2 mm or more.
  • the above hexagonal boron nitride sintered body can exhibit excellent thermal conductivity.
  • the thermal conductivity of the hexagonal boron nitride sintered body can be, for example, 20 W/mK or higher, 25 W/mK or higher, 30 W/mK or higher, or 35 W/mK or higher.
  • the above-described boron nitride sintered sheet has excellent thermal conductivity, it can be suitably used as a heat dissipation member for various devices such as semiconductor devices.
  • the adherend include a metal sheet and the like.
  • the metal sheet may be a metal plate or a metal foil.
  • Examples of the material of the metal sheet include aluminum and copper.
  • a laminate was prepared by laminating eight green sheets as described above, filled in a crucible made of boron nitride, and covered with a lid to form a closed space. This was placed in a resistance heating furnace, and the inside of the resistance heating furnace was heated from room temperature to 2200° C. at a temperature rising rate of 2° C./min under the pressure condition of atmospheric pressure in a nitrogen gas atmosphere. A sintered body was obtained by heating at 2200° C. for 5 hours. At this time, when the volume of the closed space is A [unit: L] and the total amount of the sintering aid [unit: kg] put into the closed space is B, the value of B/A is 0. The amount of sintering aid in the closed space was adjusted to 0.044 kg/L.
  • Example 2 A boron nitride sintered body sheet was obtained in the same manner as in Example 1, except that the B/A value was changed to 0.066 kg/L.
  • Example 1 A boron nitride sintered body sheet was obtained in the same manner as in Example 1, except that the heat treatment step was not performed.
  • Example 2 A boron nitride sintered body sheet was obtained in the same manner as in Example 1, except that the heat treatment step was performed in a resistance heating furnace without providing a closed space in the firing step.
  • peelability Using the sintered bodies obtained from the laminates in producing the boron nitride sintered sheets prepared in Example 1 and Comparative Example 1, the peelability was evaluated according to the following criteria. Specifically, a scraper was placed between the laminates, and evaluation was made based on the ratio of the number of sintered bodies at which the sintered bodies could be isolated without damage. Here, the "number ratio" is the number of sheets peeled off without damage/total number of sheets. From the measurement results, the peelability was evaluated according to the following criteria. Table 1 shows the results. A: The ratio of the number of sheets that can be peeled without damage is 0.75 or more.
  • B The ratio of the number of sheets that can be peeled without damage is 0.50 or more and less than 0.75.
  • C The ratio of the number of sheets that can be peeled without damage is 0.20 or more and less than 0.50.
  • D The ratio of the number of sheets that can be peeled without damage is less than 0.20.
  • Thermal conductivity H: unit W / (m K)
  • thermal diffusivity T: unit m 2 / sec
  • density D: Unit kg/m 3
  • specific heat capacity C: unit J/(kg ⁇ K)
  • a xenon flash analyzer manufactured by NETZSCH, trade name: LFA447NanoFlash
  • Density D was measured by the Archimedes method.
  • the specific heat capacity C was measured using a differential scanning calorimeter (manufactured by Rigaku Corporation, device name: ThermoPlusEvo DSC8230).

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PCT/JP2022/002676 2021-01-26 2022-01-25 窒化ホウ素焼結体シートの製造方法、及び焼結体シート Ceased WO2022163646A1 (ja)

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JPH1025296A (ja) * 1996-07-09 1998-01-27 Otsuka Chem Co Ltd 繊維状化合物及びその製造方法
JP2011178598A (ja) * 2010-03-01 2011-09-15 Hitachi Metals Ltd 窒化珪素基板の製造方法および窒化珪素基板
JP2014162697A (ja) * 2013-02-27 2014-09-08 Denki Kagaku Kogyo Kk 窒化ホウ素成形体、その製造方法及び用途
JP2015212217A (ja) * 2014-04-18 2015-11-26 株式会社トクヤマ 六方晶窒化ホウ素粉末及びその製造方法

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Publication number Priority date Publication date Assignee Title
JP2011189421A (ja) * 2010-03-12 2011-09-29 Sumitomo Electric Hardmetal Corp 立方晶窒化硼素焼結体工具
CN110168719B (zh) * 2017-03-29 2023-09-01 电化株式会社 传热构件及包含其的散热结构体

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06310822A (ja) * 1993-04-20 1994-11-04 Denki Kagaku Kogyo Kk セラミックス基板及びその用途
JPH1025296A (ja) * 1996-07-09 1998-01-27 Otsuka Chem Co Ltd 繊維状化合物及びその製造方法
JP2011178598A (ja) * 2010-03-01 2011-09-15 Hitachi Metals Ltd 窒化珪素基板の製造方法および窒化珪素基板
JP2014162697A (ja) * 2013-02-27 2014-09-08 Denki Kagaku Kogyo Kk 窒化ホウ素成形体、その製造方法及び用途
JP2015212217A (ja) * 2014-04-18 2015-11-26 株式会社トクヤマ 六方晶窒化ホウ素粉末及びその製造方法

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