WO2022210518A1 - Corps fritté en nitrure d'aluminium, procédé pour sa production, carte de circuit imprimé et substrat stratifié - Google Patents

Corps fritté en nitrure d'aluminium, procédé pour sa production, carte de circuit imprimé et substrat stratifié Download PDF

Info

Publication number
WO2022210518A1
WO2022210518A1 PCT/JP2022/014941 JP2022014941W WO2022210518A1 WO 2022210518 A1 WO2022210518 A1 WO 2022210518A1 JP 2022014941 W JP2022014941 W JP 2022014941W WO 2022210518 A1 WO2022210518 A1 WO 2022210518A1
Authority
WO
WIPO (PCT)
Prior art keywords
aluminum nitride
sintered body
nitride sintered
less
plate
Prior art date
Application number
PCT/JP2022/014941
Other languages
English (en)
Japanese (ja)
Inventor
江 尹
和久 森
勝博 小宮
Original Assignee
デンカ株式会社
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by デンカ株式会社 filed Critical デンカ株式会社
Priority to JP2023511247A priority Critical patent/JP7429825B2/ja
Publication of WO2022210518A1 publication Critical patent/WO2022210518A1/fr

Links

Images

Classifications

    • 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
    • C04B35/581—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 aluminium 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
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K1/00—Printed circuits
    • H05K1/02—Details
    • H05K1/03—Use of materials for the substrate

Definitions

  • the present disclosure relates to an aluminum nitride sintered body, a method for manufacturing the same, a circuit board, and a laminated substrate.
  • a circuit board or the like having a ceramic plate is used in such a power module in order to efficiently diffuse heat generated from a semiconductor element and to suppress leakage current.
  • a ceramic sintered body used for such a ceramic plate is generally manufactured by forming a ceramic raw material powder into a predetermined shape to form a ceramic green body, and then sintering the ceramic green body.
  • Patent Document 1 discloses that a nitride selected from the group of Zr and Ti is used in an amount of 3 to 20 parts by mass in terms of oxide as a sintering aid, and an aluminum nitride sintered body is used. Techniques for increasing the thermal conductivity and mechanical strength of steel have been proposed.
  • Electronic components such as power modules are expected to have even higher performance, and along with this, it is believed that the level of demand for the performance of various products used in electronic components will continue to rise. It is assumed that the amount of heat generated during use of electronic components will increase, and ceramic sintered bodies are also excellent in terms of withstanding the effects of differences in thermal expansion coefficients between constituent members of electronic components, that is, differences in the amount of deformation between constituent members. Bending strength is required. By using a ceramic sintered body with excellent bending strength, it may be possible to prolong the specified life of electronic components.
  • One aspect of the present disclosure is an aluminum nitride sintered body comprising aluminum nitride particles and sintering aid particles, which is laminated with a metal plate to prepare a laminate and placed in an environment of 350° C. for 5 minutes. After exposure, the above laminate was cooled in an environment of 25 ° C. for 5 minutes, and after exposing it to an environment of -78 ° C. for 5 minutes, a heat cycle test of 10 cycles was performed, with one cycle of returning to 25 ° C.
  • an aluminum nitride sintered body having an observed crack rate of less than 9.00 area % when the aluminum nitride sintered body is cracked.
  • the above-mentioned aluminum nitride sintered body can exhibit excellent bending strength because the occurrence of cracks is suppressed to a predetermined value or less when a heat cycle test is performed under specific conditions.
  • the inventors of the present invention have found through studies that if there is variation in the surface properties of the aluminum nitride sintered plate (for example, the degree of unevenness on the main surface, etc.), when an external force is applied to the aluminum nitride sintered plate, the relative It was found that stress concentration occurs in the weak part, and there may be cases where the expected bending strength is not exhibited. Furthermore, cracks that occur when a heat cycle test is performed under specific conditions are caused by aluminum nitride. It was found that the above crack rate corresponds to the development of visible cracks from latent defects in the crystal plate, and is suitable for evaluating the surface properties of aluminum nitride sintered plates. The present disclosure has been made based on the above findings.
  • the aluminum nitride sintered body has a plate shape having a pair of main surfaces, and the difference between the maximum height roughness Ry and the arithmetic mean roughness Ra on the main surfaces may be 6.00 ⁇ m or less.
  • the difference between the maximum height roughness Ry and the arithmetic mean roughness Ra is within the above range, it is possible to suppress the variation in properties on the main surface and to more uniformly disperse the thermal stress, resulting in a more excellent It can exhibit bending strength.
  • the maximum height roughness Ry may be less than 10.00 ⁇ m.
  • the particle size when the integrated value from the small particle size reaches 50% and 90% of the total is d50 and d90, respectively.
  • the value of d90-d50 may be less than 10.0 ⁇ m.
  • One aspect of the present disclosure provides a circuit board comprising the aluminum nitride sintered body described above and a conductor portion attached to the aluminum nitride sintered body.
  • the circuit board has the above-described aluminum nitride sintered body, even when the temperature during use is high, the circuit board can withstand deformation between members and exhibit excellent connection reliability.
  • One aspect of the present disclosure provides a laminated substrate comprising the aluminum nitride sintered body described above and a metal plate attached to the aluminum nitride sintered body.
  • the laminated substrate has the above-described aluminum nitride sintered body, even when the temperature during use is high, it can withstand deformation between members and can exhibit excellent connection reliability.
  • One aspect of the present disclosure is a firing step of obtaining a sintered body by firing a molded body composed of a mixture containing aluminum nitride and a sintering aid for 1 to 6 hours, and firing the sintered body at 1400 ° C. or higher and 1700 ° C.
  • a step of obtaining an annealed product by heat treatment at a temperature of less than 1 hour or more and a step of polishing the surface of the annealed product to obtain an aluminum nitride sintered body, the sintering aid
  • the agent contains yttrium oxide and aluminum oxide, the mass ratio of the aluminum oxide to the yttrium oxide is less than 0.5, and the firing step includes heating at a temperature of 1700 ° C.
  • a method of manufacturing a body is provided.
  • a sintering aid blended in a predetermined ratio is used, and the sintered body obtained by passing through at least two stages of predetermined firing processes is subjected to annealing treatment.
  • the composite compound derived from the sintering aid formed between the particles of the aluminum nitride crystals is again liquefied to promote the growth of fine aluminum nitride particles on the surface of the sintered body, and the sintered body Defects such as grain boundaries and cracks occurring on the surface are repaired, unevenness on the main surface is reduced, and then the main surface of the sintered body obtained can be made more uniform by polishing.
  • the aluminum nitride sintered body to be obtained can suppress the occurrence of stress concentration due to variations in the properties of the main surface when an external force is applied. That is, according to the manufacturing method described above, an aluminum nitride sintered body having excellent bending strength can be manufactured.
  • an aluminum nitride sintered body with excellent bending strength and a method for producing the same can be provided. According to the present disclosure, it is also possible to provide a laminated substrate and a circuit substrate that are equipped with the aluminum nitride sintered body and have excellent connection reliability.
  • FIG. 1 is a perspective view showing an example of an aluminum nitride sintered plate.
  • FIG. 2 is a perspective view showing an example of a laminated substrate.
  • FIG. 3 is a perspective view showing an example of a circuit board.
  • FIG. 4 is an SEM image showing the main surface of the annealed product and the main surface of the aluminum nitride sintered plate in the manufacturing process of the aluminum nitride sintered plate in Example 1.
  • FIG. 5 is an SEM image showing the main surface of the sintered plate before polishing and the main surface of the aluminum nitride sintered plate in the manufacturing process of the aluminum nitride sintered plate in Comparative Example 1.
  • FIG. 1 is a perspective view showing an example of an aluminum nitride sintered plate.
  • FIG. 2 is a perspective view showing an example of a laminated substrate.
  • FIG. 3 is a perspective view showing an example of a circuit board.
  • FIG. 4 is an SEM image showing the main surface of the
  • 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. .
  • FIG. 1 is a perspective view showing an example of an aluminum nitride sintered plate.
  • the aluminum nitride sintered plate 100 indicates a plate-shaped aluminum nitride sintered body having a pair of main surfaces, but its shape may be, for example, a sheet shape, and is usually a rectangular parallelepiped shape.
  • the sintering aid particles are particles containing a component derived from the sintering aid.
  • the aluminum nitride sintered plate 100 is laminated with a metal plate to prepare a laminate, exposed to a 350 ° C. environment for 5 minutes, and then cooled for 5 minutes in a 25 ° C. environment.
  • the crack rate is, for example, 8.00 area% or less, 6.00 area% or less, 5.00 area% or less, 4.00 area% or less, 3.00 area% or less, 2.00 area% or less, or It may be 1.00 area % or less.
  • the bending strength is excellent.
  • the lower limit of the crack rate is not particularly limited, it may be, for example, 0.01 area % or more.
  • the crack rate may be adjusted within the above range, and may be, for example, 0.01 to 9.00 area %.
  • the crack rate in this specification can be determined by a heat cycle test under predetermined conditions.
  • a brazing material containing silver (Ag), copper (Cu) and an active metal 90 parts by weight of Ag, 10 parts by weight of Cu, 3 parts by weight of Sn, and 3.5 parts by weight of Ti
  • a copper plate (thickness: 0.3 mm) was bonded to the aluminum nitride sintered plate 100 via a brazing material having a certain composition, so that the brazing material layer had a thickness of 15 ⁇ m.
  • a measurement sample (laminate) prepared by bonding under the conditions of 1 hour and a degree of vacuum of 1 ⁇ 10 ⁇ 3 Pa is used.
  • a crack rate is measured by a heat cycle test on the sample under predetermined conditions.
  • a specific method of the heat cycle test is as described in Examples.
  • the aluminum nitride sintered plate 100 from the viewpoint of further suppressing stress concentration and further improving bending strength, it is desirable that at least one of the opposing main surfaces is smoother, and both main surfaces are smooth. is more desirable.
  • the aluminum nitride sintered plate 100 preferably has a small difference between the maximum height roughness Ry and the arithmetic mean roughness Ra on at least one main surface.
  • the upper limit of the difference ((Ry-Ra) value) between the maximum height roughness Ry and the arithmetic mean roughness Ra on the main surface is, for example, 6.00 ⁇ m or less, 5.00 ⁇ m or less, 4.00 ⁇ m or less, 3 It may be 0.00 ⁇ m or less, 2.00 ⁇ m or less, or 1.00 ⁇ m or less.
  • the upper limit of the value of (Ry-Ra) is within the above range, it is possible to suppress the variation in properties on the main surface, disperse the thermal stress more uniformly, and improve the bending strength. can demonstrate.
  • the lower limit of the value of (Ry-Ra) is not particularly limited, and may be, for example, more than 0.01 ⁇ m or 1.00 ⁇ m or more.
  • the value of (Ry-Ra) may be adjusted within the range described above, and may be, for example, greater than 0.01 ⁇ m and 6.00 ⁇ m, or from 1.00 to 6.00 ⁇ m.
  • the upper limit of the maximum height roughness Ry of the aluminum nitride sintered plate 100 is, for example, less than 10.00 ⁇ m, 8.00 ⁇ m or less, 7.00 ⁇ m or less, 5.00 ⁇ m or less, 4.00 ⁇ m or less, 3.00 ⁇ m or less, or 2.00 ⁇ m or less.
  • the lower limit of Ry may be, for example, 0.30 ⁇ m or more, 0.60 ⁇ m or more, or 1.00 ⁇ m or more.
  • the value of the maximum height roughness Ry of the aluminum nitride sintered plate 100 may be adjusted within the above range, for example, 0.30 to 8.00 ⁇ m, 0.60 to 8.00 ⁇ m, or 1.00 to 7 00 ⁇ m.
  • the maximum height roughness Ry and the arithmetic mean roughness Ra in this specification are described in JIS B 0601: 1994 "Product Geometric Characteristics Specifications (GPS)-Surface Texture: Contour Curve Method-Terms, Definitions and Surface Texture Parameters". It means the maximum height roughness Ry and the arithmetic mean roughness Ra, which can be measured by a line contact type measuring instrument.
  • the line contact type for example, "Surface Roughness Measuring Instrument Surftest SJ-301" (product name) manufactured by Mitutoyo Co., Ltd. can be used.
  • the particle diameters when the integrated value from the small particle diameter reaches 50% and 90% of the total are d50 and d90, respectively.
  • the upper limit of the value of d90-d50 is, for example, less than 10.0 ⁇ m, 8.0 ⁇ m or less, 6.0 ⁇ m or less, 5.0 ⁇ m or less, 4.0 ⁇ m or less, 3.0 ⁇ m or less, or 2.0 ⁇ m or less. good.
  • the lower limit of the value of d90-d50 may be, for example, 0.1 ⁇ m or more, 0.5 ⁇ m or more, or 1.0 ⁇ m or more.
  • the production of the aluminum nitride sintered plate 100 can be facilitated and an increase in cost can be suppressed.
  • the upper limit of d90 of aluminum nitride particles is, for example, 15.0 ⁇ m or less, 14.0 ⁇ m or less, 13.0 ⁇ m or less, 12.0 ⁇ m or less, 11.0 ⁇ m or less, 10.0 ⁇ m or less, 9.0 ⁇ m or less, 8.0 ⁇ m or less, or 7.0 ⁇ m or less.
  • the fact that the upper limit of d90 is within the above range means that the formation of coarse particles in the aluminum nitride sintered plate 100 is suppressed, and that the structure of the sintered body is more uniform. That is, it is possible to suppress the occurrence of stress concentration when force is applied from the outside, and to further improve the bending strength of the sintered plate.
  • the lower limit of d90 may be, for example, 4.0 ⁇ m or more, 4.5 ⁇ m or more, or 5.0 ⁇ m or more.
  • d90 may be adjusted within the ranges described above, and may be, for example, 4.0 to 15.0 ⁇ m, or 5.0 to 15.0 ⁇ m.
  • d50 and d90 in this specification mean values measured by the following method.
  • the object to be measured is a position that is dug down by 50 ⁇ m from the main surface of the aluminum nitride sintered plate 100 in the thickness direction.
  • a region of 50 ⁇ m ⁇ 50 ⁇ m is determined at an arbitrary position in the acquired image, and the particle size distribution of the aluminum nitride particles is created using image analysis software.
  • the particle diameters are determined for five regions in the same manner as described above, and the arithmetic mean values are taken as the d50 and d90 of aluminum nitride, respectively.
  • the shape of the aluminum nitride particles is usually not constant. Therefore, the particle diameter of aluminum nitride particles is defined as the distance between the two most distant points on the circumference of the particle to be measured.
  • image analysis software for example, "GIMP2" (trade name) or "imageJ" (trade name) distributed under the GNU GPL can be used.
  • the upper limit of the thickness of the aluminum nitride sintered plate 100 may be, for example, 1.0 mm or less, 0.9 mm or less, 0.8 mm or less, or 0.7 mm or less. When the upper limit of the thickness is within the above range, the heat dissipation can be improved when used as a constituent member of the heat dissipation sheet.
  • the lower limit of the thickness of the aluminum nitride sintered plate 100 may be, for example, 0.15 mm or more, or 0.20 mm or more. When the lower limit of the thickness is within the above range, the heat dissipation properties and thermal resistivity of the entire circuit board prepared using the aluminum nitride sintered plate can be improved.
  • the thickness of the aluminum nitride sintered plate 100 may be adjusted within the above range, and may be, for example, 0.20-1.0 mm.
  • the aluminum nitride sintered plate 100 has excellent bending strength.
  • the bending strength of the aluminum nitride sintered plate 100 can be, for example, 370 MPa or more, 390 MPa or more, 400 MPa or more, 450 MPa or more, or 500 MPa or more.
  • Bending strength in this specification means a value measured according to the method described in JIS C 2141:1992 "Electrical insulating ceramic material test method". Specifically, it is measured according to the method described in the Examples of this specification.
  • the aluminum nitride sintered plate 100 Since the aluminum nitride sintered plate 100 has a uniform structure, the bending strength distribution is sufficiently suppressed.
  • the aluminum nitride sintered plate 100 has a relatively large Weibull coefficient in the Weibull statistical analysis of its bending strength.
  • the Weibull coefficient with respect to the bending strength of the aluminum nitride sintered plate 100 is, for example, 10.0 or more, 12.0 or more. It can be 13.0 or more, 14.0 or more, 15.0 or more, or 16.0 or more.
  • Weibull statistics are used to evaluate the distribution of flexural strength.
  • the vertical axis is the fracture probability F ( ⁇ ) and the horizontal axis is the bending strength ⁇ (strength at break, bending strength)
  • the slope m is the Weibull coefficient.
  • a large Weibull modulus means that the bending strength distribution is narrow and close to normal distribution.
  • the failure probability F( ⁇ ) in the Weibull plot is given by the following formula (1).
  • F( ⁇ ) 1 ⁇ exp[ ⁇ ( ⁇ / ⁇ ) m ] (1)
  • ⁇ is a fitting parameter.
  • the aluminum nitride sintered body described above can be produced, for example, by the following method.
  • One embodiment of a method for producing an aluminum nitride sintered body includes a firing step of obtaining a sintered body by firing a molded body composed of a mixture containing aluminum nitride and a sintering aid for 1 to 6 hours; A step of obtaining an annealed product by heat-treating the body at a temperature of 1400 ° C. or more and less than 1700 ° C. for 1 hour or more (hereinafter also referred to as an annealing step); and a step of obtaining a body (hereinafter also referred to as a polishing step).
  • Additives include binders, plasticizers, dispersion media, release agents, and the like. Binders include, for example, methylcellulose-based binders having plasticity or surfactant effects, and acrylic acid ester-based binders having excellent thermal decomposability. Examples of plasticizers include glycerin and the like. Dispersion media include, for example, ion-exchanged water and ethanol.
  • Aluminum nitride is not particularly limited, and aluminum nitride powder produced by a known method such as a direct nitriding method in which metal aluminum is nitrided in a nitrogen atmosphere, and a reduction nitriding method in which aluminum oxide is reduced with carbon. Available.
  • the sintering aid contains yttrium oxide and aluminum oxide.
  • the sintering aid may be particulate.
  • the mass ratio of aluminum oxide to yttrium oxide (content of aluminum oxide/content of yttrium oxide) is less than 0.5. Thereby, aggregation of oxides in the aluminum nitride sintered plate can be suppressed.
  • the mixing ratio of yttrium oxide and aluminum oxide can be adjusted within the range described above, thereby adjusting the oxide composition in the aluminum nitride sintered plate.
  • Aluminum oxide and yttrium oxide form a liquid phase of a composite oxide during sintering to promote sintering. Thereby, the aluminum nitride sintered plate can be sufficiently densified.
  • the content of the sintering aid may be, for example, 1 to 10.0 parts by mass with respect to 100 parts by mass of aluminum nitride.
  • the content of the sintering aid is a value calculated from the amount of the sintering aid in terms of oxide.
  • the content of aluminum oxide may be, for example, 0.1 to 5.0 parts by mass with respect to 100 parts by mass of aluminum nitride.
  • the content of aluminum oxide may be, for example, 0.1 to 5.0 parts by mass with respect to 100 parts by mass of aluminum nitride.
  • the aluminum nitride, the sintering aid, and the additive added as necessary may be blended and mixed and used as a forming raw material.
  • the forming raw material may be formed, for example, into a sheet by a known method such as a doctor blade method.
  • the molded body obtained may be degreased.
  • the degreasing method is not particularly limited, and for example, the compact may be heated to 300 to 700° C. in air or in a non-oxidizing atmosphere such as nitrogen.
  • the heating time may be, for example, 1 to 10 hours.
  • the aluminum nitride sintered body can be obtained by firing the above compact.
  • the baking step (hereinafter also referred to as the baking step) may be performed in an inert gas atmosphere.
  • the inert gas may be nitrogen, for example.
  • the firing step may be performed under atmospheric pressure.
  • the firing step includes a step of obtaining a first fired body from the molded body by heating at a temperature of 1700 ° C. or more and less than 1800 ° C. for 1 hour or more (hereinafter also referred to as a first firing step), and a temperature of 1800 to 1900 ° C. and a step of obtaining the sintered body from the first sintered body by heating at for one hour or more (hereinafter also referred to as a second sintering step).
  • firing time refers to the time during which the temperature of the atmosphere in which the object to be fired, such as the molded article, is placed reaches the firing temperature and is maintained at that temperature.
  • the firing temperature in the first firing step can be selected depending on the composition of the sintering aid, and may be, for example, 1750°C or lower, 1730°C or lower, or 1720°C or lower.
  • the rate of temperature increase until the firing temperature in the first firing step is reached may be relatively high, for example, 20° C./min or more, or 30° C./min or more.
  • the sintering temperature is preferably maintained for a predetermined period of time.
  • the firing time in the first firing step may be, for example, 1.0 hours or longer, 2.0 hours or longer, or 2.5 hours or longer.
  • the firing temperature in the second firing step may be, for example, less than 1850°C, less than 1840°C, or 1830°C or less.
  • the rate of temperature increase until reaching the firing temperature in the second firing step may be, for example, 0.5° C./min or more, or 1.0° C./min or more.
  • the sintering temperature is preferably maintained for a predetermined period of time.
  • the firing time in the second firing step may be, for example, 1.0 hours or longer, 1.5 hours or longer, or 2.0 hours or longer.
  • the firing time of the firing step is 6.0 hours or less in total, but may be, for example, 5.0 hours or less or 4.0 hours or less.
  • the total firing time of the firing step may be, for example, 1.0 hours or more, 2.0 hours or more, or 3.0 hours or more.
  • the firing time of the firing step can be adjusted within the range described above, and may be, for example, 1.0 to 4.0 hours.
  • the composite compound derived from the sintering aid formed between the grains of the aluminum nitride crystals is re-liquidized to form fine nitriding.
  • the composite compound derived from the sintering aid formed between the grains of the aluminum nitride crystals is re-liquidized to form fine nitriding.
  • Polishing is sometimes performed in the conventional method of manufacturing an aluminum nitride sintered body, but due to circumstances such as the presence of coarse particles of aluminum nitride on the surface, the unevenness before polishing is large, and it is necessary to increase the amount of polishing. If coarse particles of aluminum nitride shed from the surface during this process, large recesses may be formed. For this reason, it is not easy to smooth the surface in the conventional method of manufacturing an aluminum nitride sintered plate.
  • the aluminum nitride particles are suppressed from being coarsened and homogenized in the sintering step, and the annealing step is performed to suppress an increase in the amount of polishing and further reduce the frequency of shedding. can prepare an aluminum nitride sintered body having a smoother and more homogeneous primary surface.
  • the heating temperature in the annealing process is 1400°C or more and less than 1700°C.
  • the heating temperature in the annealing step may be, for example, 1650° C. or lower, or 1600° C. or lower.
  • the lower limit of the heating temperature in the annealing step may be, for example, 1400° C. or higher.
  • the heating temperature in the annealing step may be adjusted within the range described above, and may be, for example, 1400-1600.degree.
  • the heating time in the annealing step is 1 hour or longer, but may be 2 hours or longer, for example.
  • the upper limit of the heating time in the annealing step may be, for example, 6 hours or less.
  • the heating time in the annealing step may be adjusted within the above range, and may be, for example, 1 to 6 hours.
  • the polishing process can be performed by, for example, honing treatment.
  • the honing treatment can be performed, for example, on the surface of the annealed object under conditions of polishing pressure: 0.15 to 0.35 MPa, polishing amount: 2 to 10 ⁇ m, and time: 1 to 5 minutes.
  • the aluminum nitride sintered plate obtained by the manufacturing method described above may be processed into a desired shape as necessary.
  • the aluminum nitride sintered body may be processed into, for example, a plate having a pair of main surfaces to form an aluminum nitride sintered plate.
  • a metal part such as a metal circuit or a metal plate may be attached to the aluminum nitride sintered body to form the substrate.
  • the substrate may be, for example, a laminated substrate in which a main surface of a sintered aluminum nitride plate and a main surface of a metal plate such as a copper plate are bonded together.
  • the substrate of the present disclosure may be a laminate substrate or a circuit substrate.
  • the lower limit of the thickness of the aluminum nitride sintered body may be, for example, 0.10 mm or more, 0.20 mm or more, or 0.25 mm or more.
  • the upper limit of the thickness of the aluminum nitride sintered body may be, for example, 3.00 mm or less, 1.50 mm or less, or 1.00 mm or less.
  • the thickness of the aluminum nitride sintered body can be adjusted within the above range, and may be, for example, 0.10-3.00 mm, or 0.25-1.00 mm. By setting the thickness of the aluminum nitride sintered body within the above range, both the heat dissipation characteristics and the thermal resistivity of the entire circuit board can be achieved at higher levels.
  • FIG. 2 is a perspective view showing an example of a laminated substrate.
  • the laminated substrate 200 includes a pair of metal plates 110 arranged to face each other, and an aluminum nitride sintered plate 100 between the pair of metal plates 110 .
  • Examples of the metal plate 110 include a copper plate.
  • the shape and size of the aluminum nitride sintered plate 100 and the metal plate 110 may be the same or different.
  • the metal plate 110 and the aluminum nitride sintered plate 100 may be joined with, for example, brazing material.
  • One of the pair of metal plates 110 may be used as a heat dissipation material, and the other may be processed into a circuit pattern.
  • the circuit pattern may be formed by etching the metal plate 110 using a resist. As a result, it is possible to form a circuit board capable of sufficiently suppressing leakage current or the like, or to form a heat dissipation board.
  • FIG. 3 is a perspective view showing an example of a circuit board.
  • the circuit board 300 includes an aluminum nitride sintered plate 100 , a plurality of conductor portions 20 and a metal plate 110 .
  • Conductor portion 20 is provided on one main surface 100A of aluminum nitride sintered plate 100
  • metal plate 110 is provided on the other surface of aluminum nitride sintered plate 100 .
  • the metal plate 110 may function as a heat dissipation material.
  • the aluminum nitride sintered plate 100 in the laminated substrate 200 and the circuit board 300 is composed of an aluminum nitride sintered plate with excellent electrical insulation and thermal conductivity. Therefore, it has excellent reliability when used in various products such as power modules.
  • circuit patterns may be formed on both main surfaces of the aluminum nitride sintered plate 100 .
  • the conductor portion 20 may be formed by spraying metal powder and heat-treating it. Also, the descriptions of the above-described embodiments can be applied to each other.
  • Example 1 Production of aluminum nitride sintered plate
  • 6.0 parts by mass of yttrium oxide powder as a sintering aid and 0.3 parts by mass of ⁇ -aluminum oxide were blended and mixed using a ball mill to obtain a mixed powder.
  • cellulose ether binder manufactured by Shin-Etsu Chemical Co., Ltd., trade name: Metrose
  • glycerin manufactured by Kao Corporation, trade name: Excepar
  • ion exchange 10 parts by mass of water was added and mixed for 1 minute using a Henschel mixer to obtain a molding raw material.
  • This molding raw material is molded with a screw type extruder to produce a sheet-like molded body (width: 80 mm, thickness: 0.8 mm), dried at 100 ° C. for 1 hour, and then cut into a length of 60 mm.
  • x Width: 60 mm shaped compact was obtained.
  • boron nitride powder as a mold release agent to this compact, a plurality of the above compacts were laminated to adjust the mass of the laminate to 95 kg.
  • a degreased body was obtained by heating the obtained laminate at 600° C. in the air for degreasing.
  • the degreased body is placed in a heating furnace and heated from 25° C. to 1700° C. at a heating rate of 20° C./min under atmospheric pressure in a nitrogen gas atmosphere and held at 1700° C. for 2.5 hours. (first firing step).
  • the temperature was raised to 1820° C. at a temperature elevation rate of 1° C./min, and held at 1820° C. for 2 hours (second firing step). After that, the heating was stopped and allowed to cool in the heating furnace to obtain a sintered body.
  • An annealed product was obtained by heat-treating the sintered body at 1700°C for 2 hours in a nitrogen gas atmosphere (annealing step).
  • the surface of the annealed product is honed under the conditions of a polishing pressure of 0.15 to 0.35 MPa, a polishing amount of 2 to 10 ⁇ m, and a time of 1 to 5 minutes to obtain a thickness of 0.635 mm.
  • the aluminum nitride sintered plate was obtained (polishing step).
  • FIG. 4 shows SEM images obtained by scanning electron microscope (SEM) of the main surface of the annealed product and the main surface of the aluminum nitride sintered plate.
  • SEM scanning electron microscope
  • FIG. 4 shows the main surface of the annealed product, and (b) shows the main surface of the aluminum nitride sintered plate.
  • FIG. 4(a) shows the main surface of the annealed product
  • FIG. 4(b) shows the main surface of the aluminum nitride sintered plate.
  • a heat cycle test was performed on the obtained aluminum nitride sintered plate (thickness: 0.635 mm). Specifically, first, a brazing material containing silver (Ag), copper (Cu), and an active metal (90 parts by mass of Ag, 10 parts by mass of Cu, 3 parts by mass of Sn, and 3.5 parts by mass of Ti A copper plate (thickness: 0.3 mm) was bonded to the aluminum nitride sintered plate through a brazing material having a composition of 830° C. for a bonding time of 15 ⁇ m.
  • An aluminum nitride substrate (laminate) was prepared by bonding under the condition of vacuum degree: 1 ⁇ 10 ⁇ 3 Pa for 1 hour.
  • the obtained laminate was exposed to a 350° C. environment for 5 minutes and then cooled to a 25° C. environment for 5 minutes.
  • the laminate that has undergone the above pretreatment is first exposed to an environment in dry ice (-78 ° C.) for 5 minutes, and then returned to room temperature (25 ° C.) as one cycle.
  • a cycle test was performed. After the test, the aluminum nitride substrate was etched with an aqueous solution of copper chloride, ammonium fluoride, and hydrogen peroxide to remove the metal plate and the brazing material from the laminate, and the aluminum nitride sintered plate was taken out.
  • Example 2 An aluminum nitride sintered plate was prepared in the same manner as in Example 1, except that the annealing temperature in the annealing step was changed to 1400° C. and the annealing time was changed to 1 hour.
  • Example 3 An aluminum nitride sintered plate was prepared in the same manner as in Example 1, except that the annealing time in the annealing step was changed to 6 hours.
  • Example 4 An aluminum nitride sintered plate was prepared in the same manner as in Example 1, except that the annealing temperature in the annealing step was changed to 1500°C.
  • FIG. 5 shows SEM images obtained by a scanning electron microscope (SEM) of the main surface of the sintered body before polishing and the main surface of the aluminum nitride sintered plate.
  • SEM scanning electron microscope
  • Comparative example 2 An aluminum nitride sintered plate was prepared in the same manner as in Comparative Example 1, except that the annealing step was not performed.
  • Comparative Example 3 An aluminum nitride sintered plate was prepared in the same manner as in Comparative Example 1, except that the annealing time in the annealing step was changed to 2 hours.
  • an aluminum nitride sintered body with excellent bending strength and a method for producing the same can be provided. According to the present disclosure, it is also possible to provide a laminated substrate and a circuit substrate that are equipped with the aluminum nitride sintered body and have excellent connection reliability.
  • Conductor portion 100... Aluminum nitride sintered plate, 110... Metal plate, 200... Laminated substrate, 300... Circuit board.

Landscapes

  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Manufacturing & Machinery (AREA)
  • Ceramic Products (AREA)

Abstract

Un aspect de la présente invention concerne un corps fritté en nitrure d'aluminium qui comprend des particules de nitrure d'aluminium et des particules d'additif de frittage, le taux de fissuration observé étant inférieur à 9,00 % en surface lorsqu'un test de cycle thermique à dix cycles est réalisé sur un corps stratifié qui a été produit par stratification du corps fritté en aluminium avec une plaque métallique et qui a ensuite été soumis pendant cinq minutes à un environnement de 350°C, puis refroidi pendant cinq minutes à 25°C, chaque cycle comprenant la soumission du corps stratifié à un environnement de -78°C pendant cinq minutes puis le retour à 25°C.
PCT/JP2022/014941 2021-03-31 2022-03-28 Corps fritté en nitrure d'aluminium, procédé pour sa production, carte de circuit imprimé et substrat stratifié WO2022210518A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP2023511247A JP7429825B2 (ja) 2021-03-31 2022-03-28 窒化アルミニウム焼結体、及びその製造方法、回路基板、並びに、積層基板

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2021-060245 2021-03-31
JP2021060245 2021-03-31

Publications (1)

Publication Number Publication Date
WO2022210518A1 true WO2022210518A1 (fr) 2022-10-06

Family

ID=83456332

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/JP2022/014941 WO2022210518A1 (fr) 2021-03-31 2022-03-28 Corps fritté en nitrure d'aluminium, procédé pour sa production, carte de circuit imprimé et substrat stratifié

Country Status (2)

Country Link
JP (1) JP7429825B2 (fr)
WO (1) WO2022210518A1 (fr)

Citations (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS63129075A (ja) * 1986-11-18 1988-06-01 旭硝子株式会社 窒化アルミニウム焼結体の製造方法
JPH0524930A (ja) * 1991-07-16 1993-02-02 Showa Denko Kk ＡｌＮ焼結体およびその製造方法
JPH10245267A (ja) * 1997-03-06 1998-09-14 Denki Kagaku Kogyo Kk 窒化アルミニウム基板及びその用途
JPH10310475A (ja) * 1997-05-02 1998-11-24 Denki Kagaku Kogyo Kk 窒化アルミニウム焼結体及びその用途
JP2001097779A (ja) * 1999-09-28 2001-04-10 Toshiba Corp 窒化アルミニウム基板および同基板を用いた回路基板
JP2001102476A (ja) * 1999-09-30 2001-04-13 Toshiba Corp セラミックス基板およびその製造方法
WO2002024605A1 (fr) * 2000-09-21 2002-03-28 Sintokogio, Ltd. Procede pour renforcer une ceramique et produit ceramique
WO2002042241A1 (fr) * 2000-11-22 2002-05-30 Ibiden Co., Ltd. Corps fritte de nitrure d'aluminium, procede de production d'un corps fritte de nitrure d'aluminium, substrat ceramique et procede de production d'un substrat ceramique
JP2002293637A (ja) * 2001-03-29 2002-10-09 Denki Kagaku Kogyo Kk 窒化アルミニウム焼結体、その製造方法及び用途
JP2005075695A (ja) * 2003-09-02 2005-03-24 Denki Kagaku Kogyo Kk 窒化アルミニウム焼結体及びその製造方法
WO2006135016A1 (fr) * 2005-06-15 2006-12-21 Tokuyama Corporation Agglomere de nitrure d'aluminium, boue, objet cru, et objet degraisse
WO2007018140A2 (fr) * 2005-08-11 2007-02-15 Tokuyama Corporation Corps fritte constitue de nitrure d'aluminium
WO2017033855A1 (fr) * 2015-08-24 2017-03-02 住友電気工業株式会社 Corps fritté à base de nitrure d'aluminium et son procédé de production
WO2021261441A1 (fr) * 2020-06-22 2021-12-30 デンカ株式会社 Corps fritté en nitrure d'aluminium, substrat de circuit et substrat de jonction

Patent Citations (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS63129075A (ja) * 1986-11-18 1988-06-01 旭硝子株式会社 窒化アルミニウム焼結体の製造方法
JPH0524930A (ja) * 1991-07-16 1993-02-02 Showa Denko Kk ＡｌＮ焼結体およびその製造方法
JPH10245267A (ja) * 1997-03-06 1998-09-14 Denki Kagaku Kogyo Kk 窒化アルミニウム基板及びその用途
JPH10310475A (ja) * 1997-05-02 1998-11-24 Denki Kagaku Kogyo Kk 窒化アルミニウム焼結体及びその用途
JP2001097779A (ja) * 1999-09-28 2001-04-10 Toshiba Corp 窒化アルミニウム基板および同基板を用いた回路基板
JP2001102476A (ja) * 1999-09-30 2001-04-13 Toshiba Corp セラミックス基板およびその製造方法
WO2002024605A1 (fr) * 2000-09-21 2002-03-28 Sintokogio, Ltd. Procede pour renforcer une ceramique et produit ceramique
WO2002042241A1 (fr) * 2000-11-22 2002-05-30 Ibiden Co., Ltd. Corps fritte de nitrure d'aluminium, procede de production d'un corps fritte de nitrure d'aluminium, substrat ceramique et procede de production d'un substrat ceramique
JP2002293637A (ja) * 2001-03-29 2002-10-09 Denki Kagaku Kogyo Kk 窒化アルミニウム焼結体、その製造方法及び用途
JP2005075695A (ja) * 2003-09-02 2005-03-24 Denki Kagaku Kogyo Kk 窒化アルミニウム焼結体及びその製造方法
WO2006135016A1 (fr) * 2005-06-15 2006-12-21 Tokuyama Corporation Agglomere de nitrure d'aluminium, boue, objet cru, et objet degraisse
WO2007018140A2 (fr) * 2005-08-11 2007-02-15 Tokuyama Corporation Corps fritte constitue de nitrure d'aluminium
WO2017033855A1 (fr) * 2015-08-24 2017-03-02 住友電気工業株式会社 Corps fritté à base de nitrure d'aluminium et son procédé de production
WO2021261441A1 (fr) * 2020-06-22 2021-12-30 デンカ株式会社 Corps fritté en nitrure d'aluminium, substrat de circuit et substrat de jonction

Also Published As

Publication number Publication date
JPWO2022210518A1 (fr) 2022-10-06
JP7429825B2 (ja) 2024-02-08

Similar Documents

Publication Publication Date Title
JP5673847B2 (ja) 窒化珪素基板および窒化珪素基板の製造方法
US8858865B2 (en) Silicon nitride substrate manufacturing method, silicon nitride substrate, silicon nitride circuit substrate, and semiconductor module
TWI445682B (zh) Alumina sintered body, and its manufacturing method and semiconductor manufacturing device parts
JP6293949B2 (ja) 圧接構造用窒化珪素基板およびそれを用いた窒化珪素回路基板
JP5339214B2 (ja) 窒化珪素基板の製造方法および窒化珪素基板
JP2004260039A (ja) 半導体あるいは液晶製造装置用保持体およびそれを搭載した半導体あるいは液晶製造装置
KR101904538B1 (ko) 세라믹회로기판 및 이의 제조 방법
WO2022210518A1 (fr) Corps fritté en nitrure d'aluminium, procédé pour sa production, carte de circuit imprimé et substrat stratifié
JP7064065B1 (ja) セラミック焼結体、基板、及び、セラミック焼結体の電気絶縁性を高くする方法
JP7080422B1 (ja) 窒化アルミニウム焼結体及びその製造方法、回路基板、並びに接合基板
WO2021261452A1 (fr) Corps fritté en nitrure d'aluminium, et substrat
WO2022210520A1 (fr) Corps fritté en nitrure d'aluminium, son procédé de production, carte de circuit imprimé et substrat multicouche
JP7203286B2 (ja) 窒化アルミニウム焼結体及びその製造方法、回路基板、並びに接合基板
KR101937961B1 (ko) 평탄화 작업이 필요 없는 질화규소 기판 및 그 제조방법
JP7330416B2 (ja) 窒化アルミニウム焼結板、回路基板、並びに、積層基板
EP3846596A1 (fr) Substrat de nitrure de silicium et carte de circuit imprimé de nitrure de silicium
WO2024111483A1 (fr) Corps fritté en céramique ainsi que procédé de fabrication de celui-ci, corps lié, et module de puissance
JP2013182983A (ja) 窒化けい素回路基板およびそれを用いたモジュール
WO2024111484A1 (fr) Corps lié, et module de puissance
JP2002293641A (ja) 窒化ケイ素質焼結体
JP2000269615A (ja) 回路基板
JP3922847B2 (ja) 回路基板用窒化アルミニウム焼結体及びその製造方法
JP4868641B2 (ja) 窒化アルミニウム基板の製造方法
JP3575955B2 (ja) 放熱板
JP2022094464A (ja) 窒化シリコン用グリーンシート、および、その製造方法

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 22780729

Country of ref document: EP

Kind code of ref document: A1

ENP Entry into the national phase

Ref document number: 2023511247

Country of ref document: JP

Kind code of ref document: A

NENP Non-entry into the national phase

Ref country code: DE

122 Ep: pct application non-entry in european phase

Ref document number: 22780729

Country of ref document: EP

Kind code of ref document: A1