WO2008065980A1 - Procédé de fabrication d'un produit de jonction de nitrure d'aluminium - Google Patents

Procédé de fabrication d'un produit de jonction de nitrure d'aluminium Download PDF

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Publication number
WO2008065980A1
WO2008065980A1 PCT/JP2007/072726 JP2007072726W WO2008065980A1 WO 2008065980 A1 WO2008065980 A1 WO 2008065980A1 JP 2007072726 W JP2007072726 W JP 2007072726W WO 2008065980 A1 WO2008065980 A1 WO 2008065980A1
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Prior art keywords
aluminum nitride
nitride sintered
sintered body
bonding
paste
Prior art date
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PCT/JP2007/072726
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English (en)
Japanese (ja)
Inventor
Yukihiro Kanechika
Masanobu Azuma
Original Assignee
Tokuyama Corporation
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Filing date
Publication date
Application filed by Tokuyama Corporation filed Critical Tokuyama Corporation
Priority to JP2008546972A priority Critical patent/JP5302689B2/ja
Priority to KR1020097008605A priority patent/KR101137917B1/ko
Publication of WO2008065980A1 publication Critical patent/WO2008065980A1/fr

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    • 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
    • C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
    • 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
    • C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
    • C04B37/003—Joining burned ceramic articles with other burned ceramic articles or other articles by heating by means of an interlayer consisting of a combination of materials selected from glass, or ceramic material with metals, metal oxides or metal salts
    • C04B37/005—Joining burned ceramic articles with other burned ceramic articles or other articles by heating by means of an interlayer consisting of a combination of materials selected from glass, or ceramic material with metals, metal oxides or metal salts consisting of glass or ceramic material
    • 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
    • C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
    • C04B2237/02—Aspects relating to interlayers, e.g. used to join ceramic articles with other articles by heating
    • C04B2237/04—Ceramic interlayers
    • C04B2237/06—Oxidic interlayers
    • C04B2237/064—Oxidic interlayers based on alumina or aluminates
    • 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
    • C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
    • C04B2237/30—Composition of layers of ceramic laminates or of ceramic or metallic articles to be joined by heating, e.g. Si substrates
    • C04B2237/32—Ceramic
    • C04B2237/36—Non-oxidic
    • C04B2237/366—Aluminium nitride

Definitions

  • the present invention relates to a method for manufacturing an aluminum nitride joined body. More specifically, the present invention relates to a method for manufacturing an aluminum nitride joined body in which aluminum nitride sintered bodies are joined together.
  • semiconductor manufacturing equipment uses a member made of aluminum nitride having excellent heat resistance and corrosion resistance as a member such as a plate heater and an electrostatic chuck for mounting and processing a semiconductor wafer. It has been.
  • a member made of aluminum nitride a large member is often manufactured by joining small aluminum nitride sintered bodies to each other.
  • the base material having various shapes can be obtained from the aluminum nitride sintered body having a simple shape.
  • Patent Document 1 As shown in FIG. 5, a paste 502 containing an aluminum nitride powder and a rare earth oxide and / or calcium carbonate powder is applied on an aluminum nitride sintered body 501, After the aluminum nitride sintered body 503 is brought into intimate contact therewith, a pressure of 1 to 250 kgf / cm 2 is applied in the direction A and heated to 1700 to 2000 ° C. Is manufacturing.
  • Patent Document 2 a bonding agent containing aluminum nitride powder, alkali metal or alkaline earth metal oxide powder, and rare earth oxide powder is used, which is 5 to 500 kgf / cm 2. Under the pressure of 1400 ⁇ ; 1650 in the first step. Caro heat to C, in the second step 1650 ⁇ ; 1800. C is heated by heat to join the sintered metal bodies.
  • Patent Document 1 Japanese Patent Laid-Open No. 11 157951
  • Patent Document 2 Japanese Patent Laid-Open No. 10-273370
  • an object of the present invention is to provide a method for producing an aluminum nitride bonded body, which can firmly bond aluminum nitride sintered bodies to each other at a relatively low temperature under atmospheric pressure.
  • the method for producing an aluminum nitride joined body according to the present invention includes:
  • a paste layer containing an alkaline earth metal compound is formed on the bonding surface on which the alumina layer of one of the aluminum nitride sintered bodies is formed, and the other nitridation is performed on the paste layer. It is preferable that the step of bonding the aluminum nitride sintered bodies to each other by heating at a temperature of 1300 to 1700 ° C. after the bonding surface on which the alumina layer of the aluminum sintered body is formed is attached.
  • the thickness of the alumina layer formed on the joint surface of the aluminum nitride sintered body is preferably 0.;! To 10 ⁇ m! /.
  • aluminum nitride sintered bodies can be firmly joined to each other at a relatively low temperature under atmospheric pressure.
  • FIG. 1 is a diagram for explaining a method for producing an aluminum nitride bonded body according to the present invention.
  • FIG. 2 is a diagram for explaining a method for producing an aluminum nitride bonded body according to the present invention.
  • FIG. 3 is a diagram for explaining a method for producing an aluminum nitride bonded body according to the present invention.
  • FIG. 4 is a diagram for explaining a method for producing an aluminum nitride bonded body according to the present invention.
  • FIG. 5 is a diagram for explaining a conventional method for producing an aluminum nitride sintered body.
  • FIG. 6 is a photograph of a bonding interface in an example of the aluminum nitride bonded body of the present invention.
  • FIG. 7 is a diagram for explaining a method for measuring bonding strength.
  • FIG. 8 is a diagram for explaining a method of manufacturing a joined body in an example.
  • FIG. 9 is a diagram for explaining a method of manufacturing a joined body in an example.
  • FIG. 10 is a diagram for explaining a method of manufacturing a joined body in an example.
  • FIG. 11 is a diagram for explaining a method of manufacturing a joined body in an example.
  • a method for manufacturing an aluminum nitride bonded body according to the present invention is a method for manufacturing an aluminum nitride bonded body in which aluminum nitride sintered bodies are bonded together, wherein the two nitride layers are formed with an alumina layer formed on a bonding surface.
  • the aluminum nitride sintered bodies are heated with the aluminum sintered bodies facing each other at the joint surfaces and a paste layer containing an alkaline earth metal compound interposed between the joint surfaces. Including a joining step.
  • a paste layer containing an alkaline earth metal compound is formed on the bonding surface on which the alumina layer of one of the aluminum nitride sintered bodies is formed, and the other paste layer is formed on the paste layer.
  • heating is performed to bond the aluminum nitride sintered bodies together.
  • the alumina layer is formed on the joint surface of the aluminum nitride sintered body, so that the sintered bodies are firmly bonded to each other at a relatively low temperature and atmospheric pressure.
  • the power S can be joined.
  • the obtained joined body has high airtightness.
  • an aluminum nitride sintered body 101 in which an alumina layer 103 is formed on a joining surface 102 is prepared.
  • the shape of the aluminum nitride sintered body 101 is a plate-like force.
  • the shape is not limited to this, and may be, for example, a cylindrical shape or a polygonal column shape.
  • the aluminum nitride sintered body may have a hollow structure or a solid structure.
  • the shape of the aluminum nitride sintered body may be appropriately selected so as to obtain a desired structure of the joined body! /.
  • the relative density of the aluminum nitride sintered body 101 is preferably 97% or more.
  • the thickness of the alumina layer 103 is preferably 0.;! To 10 ⁇ m, more preferably ;! to 5 ⁇ m. If the thickness of the alumina layer is too thin, the effect of the production method of the present invention may not be obtained. If the thickness of the alumina layer is too thick, the bonding strength between the alumina layer and the aluminum nitride sintered body may be inferior.
  • the method of manufacturing the aluminum nitride sintered body 101 in which the alumina layer 103 is formed on the joint surface 102 is not particularly limited.
  • the aluminum nitride sintered body is manufactured as follows, And a method of forming an alumina layer on the surface.
  • an organic binder is added to the aluminum nitride powder, and if necessary, a sintering aid, a dispersing agent, a dispersion medium, etc. are further added and mixed. To prepare a slurry or paste.
  • Examples of the organic binder include butyral resins such as polybutyl butyral, acrylic resins such as polymethacrylol butyl, and the like.
  • the organic binder is usually used in an amount of 0.;! To 30 parts by weight, preferably 1 to 15 parts by weight per 100 parts by weight of the aluminum nitride powder.
  • alkaline earth oxides such as CaO and SrO, Y 2 O, CeO, Ho 2 O,
  • Examples include rare earth oxides such as Yb 2 O, Gd 2 O, Nd 2 O, Sm 2 O, and Dy 2 O. These
  • Y o is preferably used.
  • the sintering aid is not necessarily an oxide.
  • carbonate, nitrate, phosphate and the like may be used.
  • This sintering aid is usually used in an amount of 0.;! To 30 parts by weight, preferably 1 to 15 parts by weight per 100 parts by weight of the aluminum nitride powder.
  • Examples of the dispersant include glycerin compounds. This dispersant is usually used in an amount of 0.5;! To 10 parts by weight, preferably 0.5 to 5 parts by weight per 100 parts by weight of the aluminum nitride powder.
  • Examples of the dispersion medium include ethanol. This dispersion medium is usually used in an amount of 10 to 50 parts by weight, preferably 15 to 30 parts by weight per 100 parts by weight of the aluminum nitride powder.
  • the slurry or paste obtained as described above is formed into a desired shape.
  • it is molded by a molding means such as an extrusion molding method, an injection molding method, a swallow molding method, a doctor blade method or the like.
  • the obtained molded body is degreased and fired to produce an aluminum nitride sintered body.
  • the molding may be performed by granulating the slurry or paste with a spray dryer and then molding the granulated powder into a mold, for example, by cold isostatic pressing.
  • degreasing is preferably performed in air at 450 to 650 ° C.
  • Baking is preferably performed in a nitrogen atmosphere at 1700 to 1900 ° C.
  • the molding may be performed by a compression molding method without using an organic binder.
  • a mixed powder of aluminum nitride powder and sintering aid powder is temporarily formed with a uniaxial molding machine.
  • a green body may be produced, and a green body may be produced by pressing with a CIP (cold isostatic pressure) molding machine;! ⁇ 4t / cm 2 .
  • the degreasing step is unnecessary, and the obtained molded body is preferably fired under the conditions described above to produce an aluminum nitride sintered body.
  • the surface may be subjected to a treatment such as a roughening treatment or a polishing treatment.
  • a roughening treatment include etching with an alkaline aqueous solution and sandblasting.
  • polishing treatment include polishing using abrasive grains and electrolytic in-process dressing grinding.
  • a force for forming an alumina layer on the surface to be a bonding surface of the obtained aluminum nitride sintered body is formed by, for example, the following oxidation treatment. That is, the aluminum nitride sintered body is heated in an oxygen-containing gas atmosphere to form an alumina layer on the surface.
  • oxygen-containing gas air is the simplest force. Pure oxygen gas, oxygen is an inert gas (eg, oxygen is a rare gas such as nitrogen, carbon dioxide, argon, etc.) and / or a gas diluted with air Etc. may be used.
  • the oxygen concentration in the oxygen-containing gas is preferably 20% or more.
  • the dew point of the oxygen-containing gas is preferably ⁇ 25 ° C. or lower, more preferably ⁇ 40 ° C. to ⁇ 30 ° C.
  • the gas to be used may be dried in advance by an appropriate means such as compression or drying with a desiccant.
  • the heating temperature is usually from 1100 to 1300 ° C, preferably from 1130 to 1270 ° C, and the heating time is usually from! To 100 hours, preferably from 5 to 30 hours.
  • JP-A-2005-159334 may be used. That is, substantially dissolve oxygen during heating A process of heating the aluminum nitride sintered body to a temperature that is 300 ° C lower than the oxidation start temperature of the aluminum nitride sintered body and at a temperature equal to or higher than this temperature (this process is also simply referred to as "heating step!
  • a method including a step of forming an alumina layer by oxidizing the surface of the aluminum nitride sintered body while maintaining a high temperature (this step is also simply referred to as “oxidation step”) may be used.
  • the oxidation start temperature is 1100 ° C. under atmospheric pressure. Further, from the viewpoint of obtaining a good alumina layer, it is desirable that the temperature at which the contact with oxygen gas starts is equal to or higher than the oxidation start temperature.
  • the anolemina layer 103 may be a layer made of ⁇ -A1O.
  • the method described in JP 2001-294492 A is preferably used. Specifically, when an aluminum nitride sintered body is treated at a temperature of 800 to 1000 ° C for 0.5 to 30 hours in an oxygen atmosphere having a water vapor partial pressure of 1. OkPa or less, it is composed of ⁇ -AlO. A layer is formed.
  • FIG. 1 shows the case where the alumina layer 103 is formed only on the bonding surface 102, but the alumina layer may be formed on a surface other than the bonding surface 102 of the aluminum nitride sintered body 101. Good. That is, in the aluminum nitride sintered body 101, it is sufficient that the alumina layer 103 is formed at least on the bonding surface 102. In addition, a known method may be used to form the alumina layer 103 only on the bonding surface 102! /.
  • a paste layer 201 containing an alkaline earth metal compound is formed on the bonding surface 102 on which the anoremina layer 103 force S is formed.
  • the paste contains an alkaline earth metal compound, and preferably contains an alkaline earth metal salt or an oxide.
  • alkaline earth metal salt examples include calcium salts such as calcium carbonate and calcium nitrate. Of these, calcium carbonate is preferred.
  • alkaline earth metal oxides include calcium oxide, CaO'AlO, and 3CaO-AlO. These Lucari earth metal compounds can be used alone or in admixture of two or more.
  • the paste is usually 40 to 250 weights per 100 weight parts of the alkaline earth metal compound which may further contain aluminum oxide. Part, preferably 50 to 200 parts by weight.
  • the aluminum oxide a powder having a small particle size is preferable.
  • the paste may further contain a solvent, a dispersant and the like.
  • Examples of the solvent include turbineol. This solvent is usually used in an amount of 10 to 90 parts by weight, preferably 30 to 80 parts by weight, per 100 parts by weight of the alkaline earth metal compound powder. When the alkaline earth metal compound and aluminum oxide are included, the solvent is usually 10 to 90 parts by weight, preferably 30 to 80 parts by weight per 100 parts by weight of the total of the alkaline earth metal compound and aluminum oxide. Used in. Solvents can be used alone or in admixture of two or more.
  • Examples of the dispersant include ethylcellulose. This dispersant is usually used in an amount of 0.5 to 20 parts by weight, preferably 1 to 10 parts by weight, per 100 parts by weight of the alkaline earth metal compound powder. A dispersing agent may be used independently, or 2 or more types may be mixed and used for it.
  • the paste is obtained by adding the above components to an alkaline earth metal compound as necessary and mixing them.
  • Examples of the method for forming the layer made of the paste on the bonding surface 102 include coating and screen printing.
  • the thickness of the paste layer 201 is preferably 10 to 1000 mm, and more preferably 50 to 500 mm.
  • the bonding surface 302 on which the aluminum layer 303 of the aluminum nitride sintered body 301 is formed is attached to the paste layer 201. That is, the aluminum nitride sintered body 301 is disposed so that the bonding surface 302 formed with the alumina layer 303 of the aluminum nitride sintered body 301 is in contact with the paste layer 201.
  • the aluminum nitride sintered body 301 in which the alumina layer 303 is formed on the bonding surface 302 is the same as the aluminum nitride sintered body 101.
  • the caloric temperature is preferably 1200 to 1700. C, more preferably from 1300; C.
  • Examples of the heating atmosphere include an argon atmosphere and a nitrogen atmosphere. Nitrogen atmosphere is preferred from the viewpoint of using aluminum nitride sintered body.
  • the aluminum nitride sintered bodies can be firmly joined to each other even when heated under atmospheric pressure. Airtightness is also high. Further, in the obtained bonded body, distortion of the aluminum nitride sintered body portion that is generated when the pressure force S is not uniformly applied depending on the pressure application condition can be suppressed. Furthermore, when using a hot press sintering furnace to apply pressure with heating, it is difficult to join large sintered bodies (for example, ⁇ 500 mm or more) and sintered bodies with complex shapes. The manufacturing method of the invention has an advantage that even such sintered bodies can be easily joined.
  • the joined body may be obtained by heating at a pressure of 0.1 lMPa to 300 MPa, for example, the force with which the joined body can be obtained by heating at atmospheric pressure.
  • the heating time is preferably 1 to 30 hours, more preferably 3 to 10 hours.
  • Examples of the apparatus used for heating include an atmospheric sintering furnace, a hot press sintering furnace, and a hot isostatic press furnace.
  • the paste layer 201 is formed only on the joining surface 102 of the aluminum nitride sintered body 101 as described above.
  • a paste layer may be formed on the bonding surface 302 of the aluminum nitride sintered body 301 as well as the bonding surface 102 of the aluminum nitride sintered body 101, and the two paste layers may be adhered and subjected to heat treatment. Good.
  • the paste layer 201 is dried at a temperature of room temperature to 80 ° C, and then the bonding surface 302 on which the alumina layer 303 of the aluminum nitride sintered body 301 is formed is attached. You may let them.
  • the aluminum nitride joined body 400 obtained as described above an alumina layer is not seen in the joint portion 401, and the aluminum nitride sintered bodies are firmly joined together.
  • the joined body has high airtightness.
  • the joined portion is schematically shown in FIG. 4, since the actually obtained joined body is firmly joined, the joining interface is not usually observed in the SEM photograph. This is thought to be due to the following phenomenon occurring in the joining process. For example, when a paste containing calcium carbonate (CaCO) is used as the above paste, the calcium carbonate (CaCO) is first converted to calcium oxide (Ca) by heating.
  • CaCO calcium carbonate
  • the reason why the aluminum nitride sintered bodies can be strongly bonded to each other by heating at a relatively low temperature is considered as follows.
  • the reaction between an alkaline earth metal compound typified by calcium oxide and alumina occurs at a relatively low temperature of about 1400 ° C.
  • A1N is dissolved from the aluminum nitride particles in the calcium aluminate phase that is formed by reaction as the temperature rises.
  • the CaO—AlO—A1N produced in this way makes it possible to bond A1N firmly.
  • the aluminum nitride bonded body 400 obtained as described above is manufactured by heating at a relatively low temperature, distortion of the bonded portion 401 and the aluminum nitride sintered body portion (101, 301) is suppressed. Has been.
  • a three-point bending test was performed based on the room temperature bending test method for fine ceramics (JIS C2141). The distance between fulcrums was set to 30 mm.
  • the joined body 700 obtained by joining the aluminum nitride joined bodies 702 of 30 mm ⁇ 30 mm and 3 mm in thickness was processed into a test piece 703 having a total length of 40 mm and a thickness of 3 mm (see FIG. 7). That is, it was cut along the dotted line in FIG. Next, the test piece 703 was arranged so that the joint 701 was positioned at the center between the fulcrums, and a weight was applied from above the joint 701.
  • a 30 mm x 30 mm, 3 mm thick aluminum nitride sintered body (manufactured by Tokuyama, SH-15) was oxidized in an oxygen atmosphere at 1200 ° C for 5 hours.
  • Aluminum nitride sintered body (A— 1 1) (hereinafter referred to simply as “aluminum nitride sintered body (A— 1— 1)”) in which an alumina layer with a thickness of 2 ⁇ m is formed on the entire surface including the joint surface. I got it!
  • Sintered aluminum nitride (SH-15) made into a hollow cylinder with a diameter of 50 mm, a height of 30 mm, and a thickness of 8 mm and aluminum nitride sintered into a disk with a diameter of 50 mm and a thickness of 5 mm
  • the body made by Tokuyama, SH-15
  • each aluminum nitride sintered body (A) was formed with an alumina layer with a thickness of 2 ⁇ m on all surfaces including the joint surface.
  • — 1— 2) and (A— 1— 3) hereinafter simply referred to as aluminum nitride sintered bodies (A—1-2) and (A—1-3) respectively! /) Were obtained.
  • a 30 mm ⁇ 30 mm, 3 mm thick aluminum nitride sintered body (manufactured by Tokuyama, SH-15) was oxidized in an oxygen atmosphere at 1200 ° C. for 30 hours.
  • Aluminum nitride sintered body (A—2 1) with a 5 m thick alumina layer formed on the surface of all surfaces including the joint surface (hereinafter referred to simply as aluminum nitride sintered body (A—2-1))! /, U got.
  • Aluminum nitride sintered body (made by Tokama, SH-15) processed into a hollow cylindrical shape with a diameter of 50 mm, a height of 30 mm, and a thickness of 8 mm and aluminum nitride sintered into a disk with a diameter of 50 mm and a thickness of 5 mm
  • the body (made by Tokuyama, SH-15) was oxidized in the same way, and each of the aluminum nitride sintered bodies (A— 2-2) and (A-2-3) (hereinafter also referred to simply as aluminum nitride sintered bodies (A-2-2) and (A-2-3), respectively) were obtained.
  • Aluminum nitride sintered body (B—1 1) (hereinafter simply referred to as “aluminum nitride sintered body (B—1 1)”) in which an alumina layer having a thickness of 2 ⁇ m is formed on the entire surface including the joint surface. )
  • Aluminum nitride sintered body (SH-50) made into a hollow cylinder with ⁇ 50mm, height 30mm, thickness 8mm and aluminum nitride sintered into ⁇ 50mm, thickness 5mm disc
  • the body made by Tokuyama, SH-50
  • — 1 2) and (B— 1 3) hereinafter also referred to simply as aluminum nitride sintered bodies (B— 1 2) and (B— 1— 3), respectively) were obtained.
  • a 30 mm ⁇ 30 mm, 3 mm thick aluminum nitride sintered body (manufactured by Tokuyama, SH-15) was oxidized in an oxygen atmosphere at 1100 ° C. for 2 hours.
  • Aluminum nitride sintered body (A— 3— 1) in which an alumina layer with a thickness of 0.5 111 is formed on the entire surface including the joint surface (hereinafter simply referred to as “aluminum nitride sintered body (A— 3 1)”) Also called).
  • Aluminum nitride sintered body (made by Tokama, SH-15) processed into a hollow cylindrical shape with a diameter of 50 mm, a height of 30 mm, and a thickness of 8 mm and aluminum nitride sintered into a disk with a diameter of 50 mm and a thickness of 5 mm
  • the body (made by Tokuyama, SH-15) was also oxidized in the same manner, and each of the surfaces including the joint surface was formed with an aluminum nitride sintered body (0.5 m thick alumina layer).
  • A—3—2) and (A—3—3) hereinafter referred to simply as aluminum nitride sintered bodies (A—3—2) and (A—3—3), respectively)! It was.
  • a 30 mm ⁇ 30 mm, 3 mm thick aluminum nitride sintered body (manufactured by Tokuyama, SH-15) was oxidized in an oxygen atmosphere at 1300 ° C. for 15 hours.
  • Aluminum nitride sintered body (A—41) (hereinafter also referred to simply as “aluminum nitride sintered body (A—41))” with an alumina layer of 7 m thickness formed on all surfaces including the joint surface Got.
  • Aluminum nitride sintered bodies (A—4—2) and (A—4—3) (hereinafter referred to simply as aluminum nitride sintered bodies, respectively) in which an alumina layer having a thickness of 7 m is formed on the entire surface. (A-4-2) and (A-4-3)) were obtained.
  • a bonding paste (A) was prepared by mixing 50 g of calcium carbonate (manufactured by Wako Pure Chemical Industries, Ltd.) and 50 g of alumina powder (manufactured by Showa Denko) with 60 g of turbineol as a solvent and 3 g of ethylcellulose as a dispersant using a ball mill. .
  • a bonding paste (B) was prepared by mixing 100 g of calcium carbonate (manufactured by Wako Pure Chemical Industries, Ltd.), 60 g of turbineol as a solvent, and 3 g of ethylcellulose as a dispersant using a ball mill.
  • a bonding paste (C) was prepared by mixing 3 g of 3CaO 2 —Al 2 O 3 as a solvent, 60 g of terbinol as a solvent, and 3 g of ethyl cell mouth as a dispersant using a ball mill.
  • a bonding paste (D) was prepared by mixing 100 g of calcium oxide (manufactured by Wako Pure Chemical Industries, Ltd.), 60 g of terbeneol as a solvent, and 3 g of ethylcellulose as a dispersant using a ball mill.
  • the bonding paste (A) was applied to the aluminum nitride sintered body (A— 1-1) to a thickness of 300 m, and another aluminum nitride sintered body (A— 1-1) was applied to the applied bonding paste (A) layer. 1) was installed (see Figs. 8 and 9).
  • This aluminum nitride sintered body (A-1-1) (with another aluminum nitride sintered body (A-1-1) placed) is maintained at 80 ° C
  • a drying treatment was applied in the inside. Next, this is placed in a boron nitride jig and heated in a nitrogen atmosphere at 1600 ° C for 5 hours to produce the same aluminum nitride sintered body (A-1-1). Joined.
  • the bonding paste (A) is applied to the aluminum nitride sintered body (A—1-2) to a thickness of 300 m, and the aluminum nitride sintered body (A—13) is placed on the applied bonding paste (A) layer.
  • the aluminum nitride sintered body (A-12) (with the aluminum nitride sintered body (A-13) placed thereon) was subjected to a drying treatment in a constant temperature dryer maintained at 80 ° C. did. Next, both were joined by heating under the same conditions as in Example 11-1.
  • the leak amount was 5. ⁇ ⁇ ⁇ tm'cc / sec or less, indicating high airtightness.
  • the leak amount was 5. ⁇ ⁇ ⁇ tm'cc / sec or less, which showed high hermeticity.
  • Bonding was performed in the same manner as in Example 1-2.
  • Bonding was performed in the same manner as in Example 11 except that the bonding paste (B) was used instead of the bonding paste (A). As a result of the bending strength test of this joined body, it showed the same strength (330 MPa) as the aluminum nitride sintered body before joining.
  • Bonding was performed in the same manner as in Example 12 except that the bonding paste (B) was used instead of the bonding paste (A).
  • the leak amount was 5. ⁇ ⁇ ⁇ tm'cc / sec or less, indicating high airtightness.
  • Bonding was performed in the same manner as in Example 1-1, except that the bonding paste (C) was used instead of the bonding paste (A). As a result of the bending strength test of this joined body, it showed the same strength (330 MPa) as the sintered aluminum nitride before joining.
  • Bonding was performed in the same manner as in Example 12 except that the bonding paste (C) was used instead of the bonding paste (A).
  • Joining was performed in the same manner as in Example 1-2, except that the joining paste (D) was used instead of the joining paste (A).
  • the leak amount was 5. ⁇ ⁇ ⁇ tm'cc / sec or less, which showed high hermeticity.
  • Joining was performed in the same manner as in Example 1-1, except that the aluminum nitride sintered body (A-3 1) was used instead of the aluminum nitride sintered body (A-11). As a result of the bending strength test of this joined body, it showed the same strength (320 MPa) as the aluminum nitride sintered body before joining.
  • Aluminum nitride sintered bodies (A—4-2—) and (A—4-3) are used instead of aluminum nitride sintered bodies (A—1-2) and (A—1-3)! Except for the above, joining was performed in the same manner as in Example 12.

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Abstract

Cette invention concerne un procédé de fabrication d'un produit de jonction de nitrure d'aluminium comprenant des frittes de nitrure d'aluminium réunies entre elles. Le procédé de fabrication est caractérisé par le fait qu'il comprend l'étape consistant à disposer deux frittes de nitrure d'aluminium ayant une couche d'alumine sur leurs faces de jonction, de telle sorte que les faces de jonction sont tournées l'une vers l'autre, interposer une couche de pâte contenant un composé de métal alcalino-terreux entre les faces de jonction, et à chauffer l'ensemble dans cet état à une température de 1 300 à 1 700°C pour réunir les frittes de nitrure d'aluminium entre elles.
PCT/JP2007/072726 2006-11-27 2007-11-26 Procédé de fabrication d'un produit de jonction de nitrure d'aluminium WO2008065980A1 (fr)

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JP2019026511A (ja) * 2017-07-31 2019-02-21 日本特殊陶業株式会社 セラミックス接合体およびセラミックス接合体の製造方法

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JP2019026511A (ja) * 2017-07-31 2019-02-21 日本特殊陶業株式会社 セラミックス接合体およびセラミックス接合体の製造方法

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JPWO2008065980A1 (ja) 2010-03-04
KR101137917B1 (ko) 2012-05-09

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