JP2002293641A - Silicon nitride-based sintered compact - Google Patents
Silicon nitride-based sintered compactInfo
- Publication number
- JP2002293641A JP2002293641A JP2001096497A JP2001096497A JP2002293641A JP 2002293641 A JP2002293641 A JP 2002293641A JP 2001096497 A JP2001096497 A JP 2001096497A JP 2001096497 A JP2001096497 A JP 2001096497A JP 2002293641 A JP2002293641 A JP 2002293641A
- Authority
- JP
- Japan
- Prior art keywords
- silicon nitride
- sintered body
- thermal conductivity
- room temperature
- based sintered
- Prior art date
- Legal status (The legal status 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 status listed.)
- Granted
Links
- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 65
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 65
- 239000002245 particle Substances 0.000 claims description 12
- 238000005245 sintering Methods 0.000 claims description 11
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 10
- 239000000395 magnesium oxide Substances 0.000 claims description 10
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 10
- 239000000758 substrate Substances 0.000 claims description 10
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 9
- 238000013001 point bending Methods 0.000 claims description 8
- 150000004767 nitrides Chemical class 0.000 claims description 3
- 230000001747 exhibiting effect Effects 0.000 abstract 1
- 239000004065 semiconductor Substances 0.000 description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000000465 moulding Methods 0.000 description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 3
- 230000017525 heat dissipation Effects 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 238000005219 brazing Methods 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 239000011362 coarse particle Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000011812 mixed powder Substances 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 238000007088 Archimedes method Methods 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000007606 doctor blade method Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000005121 nitriding Methods 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000005382 thermal cycling Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
Landscapes
- Ceramic Products (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、窒化ケイ素を主成
分する窒化ケイ素質焼結体に係り、特に高密度、高強
度、高熱伝導率で絶縁基板および回路基板として用いる
のに好適な窒化ケイ素質焼結体に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a silicon nitride sintered body containing silicon nitride as a main component, and more particularly to a silicon nitride sintered body having a high density, a high strength and a high thermal conductivity and suitable for use as an insulating substrate and a circuit substrate. It relates to an elementary sintered body.
【０００２】[0002]
【従来の技術】窒化ケイ素質焼結体は、強度や靭性に優
れるため各種機械部品に用いられるほか、高い絶縁性を
利用して電気絶縁材料にも適用されている。従来の電気
絶縁セラミックスとして、酸化アルミニウム、窒化アル
ミニウムなどがある。酸化アルミニウムは熱伝導率が低
いため、近年特に発展の著しいパワー半導体などへの適
用に対して放熱性が不足する問題がある。また、窒化ア
ルミニウムは熱伝導率が高く放熱性に優れるが、機械的
強度や破壊靭性が低いため、モジュールの組み立て工程
での締め付け工程で割れを生じたり、半導体素子を実装
した回路基板では半導体素子との熱膨張差に起因して熱
サイクルによりクラックや割れを生じ実装信頼性が低下
する問題がある。2. Description of the Related Art A silicon nitride sintered body is used for various mechanical parts because of its excellent strength and toughness, and is also applied to an electrical insulating material by utilizing its high insulating property. Conventional electric insulating ceramics include aluminum oxide and aluminum nitride. Since aluminum oxide has a low thermal conductivity, there is a problem that heat dissipation is insufficient for application to power semiconductors and the like, which have been particularly remarkable in recent years. Aluminum nitride has high thermal conductivity and excellent heat dissipation, but its mechanical strength and fracture toughness are low, so cracks may occur in the fastening process in the module assembly process, or semiconductor devices may be used in circuit boards on which semiconductor devices are mounted. There is a problem that cracks and cracks are caused by thermal cycling due to the difference in thermal expansion between them and the mounting reliability is reduced.
【０００３】そこで、電気絶縁セラミックスとして強度
および靭性に優れる窒化ケイ素を利用した種々の提案が
ある。例えば、特開平４−１７５２６８号には焼結体密
度が３．１５ｇ／ｃｍ3以上で、熱伝導率が４０Ｗ／
（ｍ・Ｋ）以上の窒化ケイ素質焼結体が記載されてい
る。また、特開平１１−１００２７６号には破壊靭性が
６ＭＰａ√ｍ以上、熱伝導率が６０Ｗ／（ｍ・Ｋ）の窒
化ケイ素質焼結体が記載されている。[0003] Therefore, there are various proposals utilizing silicon nitride having excellent strength and toughness as an electrically insulating ceramic. For example, Japanese Patent Application Laid-Open No. 4-175268 discloses that a sintered body has a density of 3.15 g / cm 3 or more and a thermal conductivity of 40 W /
A silicon nitride based sintered body of (m · K) or more is described. Japanese Patent Application Laid-Open No. H11-100276 describes a silicon nitride sintered body having a fracture toughness of 6 MPaＭＰm or more and a thermal conductivity of 60 W / (m · K).
【０００４】[0004]
【発明が解決しようとする課題】しかしながら、これら
従来の窒化ケイ素質焼結体は近年益々発熱量が増大する
半導体モジュールに対しては熱伝導率が不足しがちであ
り、特に動作中の高温域まで放熱性を安定に確保するこ
とがより一層望まれている。本発明はかかる事情に鑑
み、高密度、高強度、高熱伝導の窒化ケイ素質焼結体を
提供することを目的とする。However, these conventional silicon nitride sintered bodies tend to have a shortage of thermal conductivity with respect to semiconductor modules which generate more and more heat in recent years. It is even more desired to ensure stable heat dissipation. In view of such circumstances, an object of the present invention is to provide a silicon nitride sintered body having high density, high strength, and high thermal conductivity.
【０００５】[0005]
【課題を解決するための手段】本発明の窒化ケイ素質焼
結体は、熱伝導率が室温において７５Ｗ／（ｍ・Ｋ）以
上であり、かつ室温から２００℃までにおいて４５Ｗ／
（ｍ・Ｋ）以上であることを特徴とする。The silicon nitride sintered body of the present invention has a thermal conductivity of 75 W / (m · K) or more at room temperature and 45 W / (m · K) from room temperature to 200 ° C.
(M · K) or more.
【０００６】本発明において、窒化ケイ素質焼結体が窒
化ケイ素粉末に焼結助剤として酸化物、窒化物または酸
窒化物の１種以上を６ｗｔ％以下添加した後、焼結され
たものであって、相対密度が９７％以上であり、室温に
おいて３点曲げ強度が８００ＭＰａ以上であることを特
徴とする。In the present invention, a silicon nitride sintered body is obtained by adding at least one of oxide, nitride or oxynitride as a sintering aid to silicon nitride powder in an amount of 6 wt% or less and then sintering. The relative density is 97% or more, and the three-point bending strength at room temperature is 800 MPa or more.
【０００７】また、本発明において、窒化ケイ素質焼結
体が窒化ケイ素粉末に焼結助剤として酸化マグネシウム
および／または酸化イットリウムを６ｗｔ％以下添加し
た後、焼結されたものであって、その添加量が重量比
で、酸化マグネシウム／酸化イットリウム≦３．０を満
足することを特徴とする。In the present invention, the silicon nitride sintered body is obtained by adding magnesium oxide and / or yttrium oxide as a sintering aid to a silicon nitride powder in an amount of 6 wt% or less and then sintering the silicon nitride powder. It is characterized in that the addition amount satisfies magnesium oxide / yttrium oxide ≦ 3.0 in weight ratio.
【０００８】さらに、本発明において、窒化ケイ素質焼
結体の切断面を観察したとき、柱状のβ型窒化ケイ素粒
子の内、長軸の長さが１０μｍを超えるものが、１ｍｍ
2当たりに２００００個以下であることを特徴とする。Further, in the present invention, when observing the cut surface of the silicon nitride based sintered body, it was found that among the columnar β-type silicon nitride particles, those having a major axis length exceeding 10 μm were 1 mm.
It is characterized in that 20,000 or less per 2 pieces.
【０００９】[0009]
【作用】窒化ケイ素質焼結体は、その内部に存在する異
なるイオンによるフォノン散乱により熱伝導率が低下す
る。また、窒化ケイ素質焼結体は、窒化ケイ素粒子相と
その粒界相とから構成され、この粒界相量が増えるにし
たがい熱伝導率が低下する。また、窒化ケイ素質焼結体
内に残存する気孔は熱伝導率を低下させるので緻密な焼
結体であることが必要である。このため、窒化ケイ素質
焼結体が室温において７５Ｗ／（ｍ・Ｋ）以上、室温か
ら２００℃までにおいて４５Ｗ／（ｍ・Ｋ）以上の高熱
伝導率を得るためには、窒化ケイ素粉末に焼結助剤とし
て酸化物、窒化物または酸窒化物の１種以上を６ｗｔ％
以下、さらに好ましくは、焼結助剤として酸化マグネシ
ウムおよび／または酸化イットリウムを６ｗｔ％以下で
その添加量が重量比で、酸化マグネシウム／酸化イット
リウム≦３．０を満足するように添加した後、相対密度
が９７％以上の焼結体にする。The thermal conductivity of a silicon nitride sintered body is reduced due to phonon scattering caused by different ions present inside the sintered body. Further, the silicon nitride sintered body is composed of a silicon nitride particle phase and its grain boundary phase, and the thermal conductivity decreases as the amount of the grain boundary phase increases. Further, the pores remaining in the silicon nitride sintered body reduce the thermal conductivity, so that the sintered body needs to be a dense sintered body. Therefore, in order to obtain a silicon nitride-based sintered body having a high thermal conductivity of 75 W / (m · K) or more at room temperature and 45 W / (m · K) or more from room temperature to 200 ° C., the silicon nitride powder needs to be sintered. 6 wt% of one or more of oxide, nitride or oxynitride as a binder
Hereafter, more preferably, magnesium oxide and / or yttrium oxide are added as a sintering aid in an amount of 6 wt% or less so that the addition amount satisfies magnesium oxide / yttrium oxide ≦ 3.0 by weight. The sintered body has a density of 97% or more.
【００１０】また、窒化ケイ素質焼結体中の窒化ケイ素
粒子の性状を最適化することにより曲げ強度を高めるこ
とができる。本発明の窒化ケイ素質焼結体のミクロ組織
は、マトリックスに良熱伝導体である粒子の長軸長さが
１０μｍ以上である柱状のβ型窒化ケイ素粒子を含んで
いる。走査型電子顕微鏡等で窒化ケイ素質焼結体の切断
面を観察したとき、柱状のβ型窒化ケイ素粒子の内、長
軸の長さが１０μｍを超えるものが、１ｍｍ2当たりに
２００００個を超える場合、組織中に導入されたこの粗
大粒子が破壊の起点として作用するために破壊靭性が大
きく低下し、室温における３点曲げ強度が８００ＭＰａ
未満となり不十分である。The bending strength can be increased by optimizing the properties of the silicon nitride particles in the silicon nitride sintered body. The microstructure of the silicon nitride-based sintered body of the present invention includes columnar β-type silicon nitride particles having a major axis length of 10 μm or more as a good heat conductor in a matrix. When observing the cross section of the silicon nitride sintered body with a scanning electron microscope or the like, among the columnar β-type silicon nitride particles, those having a major axis length of more than 10 μm exceed 20,000 per 1 mm 2 In this case, since the coarse particles introduced into the structure act as starting points of fracture, the fracture toughness is greatly reduced, and the three-point bending strength at room temperature is 800 MPa.
Less than that is insufficient.
【００１１】[0011]
【発明の実施の形態】第１の実施例 焼結助剤として平均粒子径０．２μｍの酸化マグネシウ
ム（ＭｇＯ）粉末、平均粒子径０．３μｍの酸化イット
リウム（Ｙ2Ｏ3）粉末を用意した。ついで、平均粒子径
０．５μｍの窒化ケイ素（Ｓｉ3Ｎ4）粉末に前記焼結助
剤を所定量添加し、エタノール中でボールミルなどを用
いて粉砕、混合を行った。そして、真空乾燥後、篩いを
通して造粒し、得られた混合粉末をＣＩＰ成形またはシ
ート成形により成形し成形体を得た。さらに、得られた
成形体を１７００〜２０００℃、９〜２０００気圧の窒
素ガス雰囲気中で焼結し、数種類の窒化ケイ素質焼結体
を作製した。DESCRIPTION OF THE PREFERRED EMBODIMENTS First Embodiment Magnesium oxide (MgO) powder having an average particle diameter of 0.2 μm and yttrium oxide (Y 2 O 3 ) powder having an average particle diameter of 0.3 μm were prepared as sintering aids. . Subsequently, a predetermined amount of the sintering aid was added to silicon nitride (Si 3 N 4 ) powder having an average particle diameter of 0.5 μm, and the mixture was pulverized and mixed in ethanol using a ball mill or the like. Then, after vacuum drying, the mixture was granulated through a sieve, and the obtained mixed powder was molded by CIP molding or sheet molding to obtain a molded body. Further, the obtained molded body was sintered in a nitrogen gas atmosphere at 1700 to 2000 ° C. and 9 to 2000 atm to produce several types of silicon nitride sintered bodies.
【００１２】得られた窒化ケイ素質焼結体から、直径１
０ｍｍ×厚さ３ｍｍの熱伝導率および密度測定用の試験
片、縦３ｍｍ×横４ｍｍ×長さ４０ｍｍの３点曲げ試験
片を採取した。熱伝導率はレーザーフラッシュ法により
室温で測定した。密度はアルキメデス法により窒化ケイ
素質焼結体の真密度を配合組成から求め、測定値を真密
度で除することにより相対密度を求めた。３点曲げ強度
は室温で３点抗折試験を行い測定した。From the obtained silicon nitride sintered body, a diameter of 1
A test piece of 0 mm × thickness 3 mm for measuring thermal conductivity and density and a three-point bending test piece of 3 mm long × 4 mm wide × 40 mm long were collected. Thermal conductivity was measured at room temperature by the laser flash method. For the density, the true density of the silicon nitride sintered body was determined from the composition by the Archimedes method, and the relative density was determined by dividing the measured value by the true density. The three-point bending strength was measured by performing a three-point bending test at room temperature.
【００１３】また、ＳＥＭを用いて倍率５００倍にて、
窒化ケイ素質焼結体の切断面の１ｍｍ2の領域を任意に
３箇所観察し、その領域中に存在する長軸の長さが１０
μｍを超える柱状のβ型窒化ケイ素粒子の個数を調べ、
その平均値を求めた。Further, at 500 × magnification using SEM,
An area of 1 mm 2 of the cut surface of the silicon nitride sintered body optionally three observation, the length of the long axis present in that area 10
Check the number of columnar β-type silicon nitride particles exceeding μm,
The average was determined.
【００１４】その測定結果を表１および表２に示す。表
１および表２において、試料Ｎｏ．１〜７は本発明例で
あり、試料Ｎｏ．１１〜１６は比較例であり、室温での
曲げ強度とは３点曲げ強度、粗大粒子個数とは窒化ケイ
素質焼結体の切断面の１ｍｍ 2の領域において、粒子の
長軸の長さが１０μｍを超えるβ型窒化ケイ素粒子の個
数を表わす。Tables 1 and 2 show the measurement results. table
In Table 1 and Table 2, Sample No. 1 to 7 are examples of the present invention.
Yes, sample No. 11 to 16 are comparative examples, which were obtained at room temperature.
The bending strength is three-point bending strength, and the number of coarse particles is silicon nitride.
1mm of cut surface of base sintered body TwoIn the region of
Β-type silicon nitride particles whose major axis exceeds 10 μm
Represents a number.
【００１５】[0015]
【表１】 [Table 1]
【００１６】[0016]
【表２】 [Table 2]
【００１７】表１および表２の結果から、本発明例は、
焼結助剤の酸化マグネシウムおよび酸化イットリウムの
合計添加量が６ｗｔ％以下で、その添加量が重量比で、
酸化マグネシウム／酸化イットリウム≦３．０を満足す
る。さらに、窒化ケイ素質焼結体内の長軸の長さが１０
μｍを超える柱状のβ型窒化ケイ素粒子が１ｍｍ2当た
りに２００００個以下含まれ、相対密度が９７％以上で
あるため、室温において熱伝導率が７５Ｗ／（ｍ・Ｋ）
以上、３点曲げ強度が８００ＭＰａ以上を得ることがで
きた。From the results in Tables 1 and 2, the present invention example
The total added amount of magnesium oxide and yttrium oxide as sintering aids is 6 wt% or less, and the added amount is
Satisfies magnesium oxide / yttrium oxide ≦ 3.0. Furthermore, the length of the long axis in the silicon nitride sintered body is 10
Since 20,000 or less columnar β-type silicon nitride particles exceeding 1 μm are contained per 1 mm 2 and the relative density is 97% or more, the thermal conductivity at room temperature is 75 W / (m · K).
As described above, a three-point bending strength of 800 MPa or more was obtained.
【００１８】また、図１は本発明例（試料Ｎｏ．６）の
窒化ケイ素質焼結体における室温から２００℃までの熱
伝導率の変化を示す。本発明例では、熱伝導率が室温に
おいて８３Ｗ／（ｍ・Ｋ）、１００℃において７４Ｗ／
（ｍ・Ｋ）、２００℃において６２Ｗ／（ｍ・Ｋ）であ
り、絶縁基板などで通常使用される約２００℃の温度域
まで高い熱伝導率を確保し、安定した放熱性を発揮でき
る。本発明の窒化ケイ素質焼結体は、室温から２００℃
までにおいて熱伝導率が４５Ｗ／（ｍ・Ｋ）以上である
ことが好ましい。より好ましくは、室温から２００℃ま
でにおいて熱伝導率が５０Ｗ／（ｍ・Ｋ）以上である。FIG. 1 shows a change in thermal conductivity from room temperature to 200 ° C. in the silicon nitride sintered body of the example of the present invention (sample No. 6). In the example of the present invention, the thermal conductivity is 83 W / (m · K) at room temperature and 74 W / (m · K) at 100 ° C.
(M · K), which is 62 W / (m · K) at 200 ° C., ensuring a high thermal conductivity up to a temperature range of about 200 ° C. usually used for an insulating substrate or the like, and can exhibit stable heat radiation. The silicon nitride-based sintered body of the present invention has a temperature from room temperature to 200 ° C.
Up to 45 W / (m · K) or more. More preferably, the thermal conductivity from room temperature to 200 ° C. is 50 W / (m · K) or more.
【００１９】第２の実施例 窒化ケイ素粉末に所定量の焼結助剤を添加した混合粉末
を、アミン系の分散剤を所定量添加したトルエン・ブタ
ノール溶液中に挿入し、樹脂製ポットならびに窒化ケイ
素製ボールを加え２４時間湿式混合した後、結合剤およ
び可塑剤を加え更に２４時間混合して成形用スラリーを
得た。この成形用スラリーを粘度調整した後、ドクター
ブレード法によりグリーンシートを作製した。次に、得
られたグリーンシートを空気中、４００〜６００℃で１
〜２時間加熱し、予め添加していた有機バインダー成分
を除去した。そして、このシートを所定の条件で焼成
し、本発明の特徴を有する窒化ケイ素質焼結体を得た。
この窒化ケイ素質焼結体を機械加工し、寸法５０ｍｍ×
５０mm×厚さ０．８ｍｍの半導体装置用絶縁基板を製造
した。Second Embodiment A mixed powder obtained by adding a predetermined amount of a sintering aid to a silicon nitride powder was inserted into a toluene / butanol solution containing a predetermined amount of an amine-based dispersant, and a resin pot and a nitriding solution were added. After adding a silicon ball and performing wet mixing for 24 hours, a binder and a plasticizer were added and mixed for another 24 hours to obtain a molding slurry. After adjusting the viscosity of the molding slurry, a green sheet was prepared by a doctor blade method. Next, the obtained green sheet is heated at 400 to 600 ° C. in air for 1 hour.
The mixture was heated for ~ 2 hours to remove the organic binder component added in advance. Then, the sheet was fired under predetermined conditions to obtain a silicon nitride sintered body having the features of the present invention.
This silicon nitride sintered body was machined to a size of 50 mm ×
A 50 mm × 0.8 mm thick insulating substrate for a semiconductor device was manufactured.
【００２０】この窒化ケイ素質焼結体製絶縁基板を用い
て、図２に示すような回路基板を作製した。図２におい
て、本発明例の回路基板１は窒化ケイ素質焼結体製絶縁
基板２の表面に銅回路板３を裏面に銅板４をろう材５に
より接合して構成される。A circuit board as shown in FIG. 2 was manufactured using the insulating substrate made of a silicon nitride sintered body. In FIG. 2, a circuit board 1 according to the present invention is formed by bonding a copper circuit board 3 to a front surface of an insulating substrate 2 made of a silicon nitride sintered body and a copper plate 4 to a back surface thereof by a brazing material 5.
【００２１】得られた本発明の回路基板に対して耐熱サ
イクル試験を行った。耐熱サイクル試験は、−４０℃で
の冷却を２０分、室温での保持を１０分及び１８０℃に
おける加熱を２０分とする昇温・降温サイクルを１サイ
クルとし、これを繰り返し付与し、基板部に亀裂などが
発生するまでのサイクル数を測定した。その結果、１０
００サイクル経過後においても、窒化ケイ素質焼結体製
基板に亀裂など発生せず、耐久性に優れることが確認で
きた。The obtained circuit board of the present invention was subjected to a heat cycle test. In the heat cycle test, the heating and cooling cycle in which cooling at −40 ° C. was 20 minutes, holding at room temperature for 10 minutes, and heating at 180 ° C. for 20 minutes was one cycle, and the cycle was repeatedly applied. The number of cycles up to the occurrence of cracks was measured. As a result, 10
Even after the lapse of 00 cycles, it was confirmed that the substrate made of the silicon nitride-based sintered body did not crack or the like and was excellent in durability.
【００２２】[0022]
【発明の効果】本発明の窒化ケイ素質焼結体は、高強度
・高靭性に加え高い熱伝導率が付与されるため、半導体
素子用絶縁基板として用いた場合、耐久性に優れた基板
材料となる。また、高強度と高熱伝導率を両立できるた
め、耐熱衝撃性が必要とされる機械構造部品にも適用で
きる。The silicon nitride sintered body of the present invention is provided with a high thermal conductivity in addition to high strength and high toughness. Therefore, when used as an insulating substrate for a semiconductor device, the substrate material has excellent durability. Becomes Further, since both high strength and high thermal conductivity can be achieved, the present invention can be applied to mechanical structural parts requiring thermal shock resistance.
【図１】本発明例の窒化ケイ素質焼結体の室温から２０
０℃までの熱伝導率の変化を示す。FIG. 1 shows that the silicon nitride-based sintered body of the present invention has a temperature from room temperature to 20 ° C.
The change in thermal conductivity up to 0 ° C. is shown.
【図２】本発明例の窒化ケイ素質焼結体製回路基板の断
面図を示す。FIG. 2 is a sectional view of a circuit board made of a silicon nitride sintered body of the present invention.
１ 回路基板 、２ 基板、３ 銅回路板、４ 銅板、
５ ろう材1 circuit board, 2 board, 3 copper circuit board, 4 copper board,
5 brazing filler metal
───────────────────────────────────────────────────── フロントページの続き Ｆターム(参考） 4G001 BA06 BA09 BA32 BB06 BB09 BB32 BC23 BD03 BD14 BD23 BE03 BE21 BE23 BE32 BE33 ──────────────────────────────────────────────────続 き Continued on the front page F term (reference) 4G001 BA06 BA09 BA32 BB06 BB09 BB32 BC23 BD03 BD14 BD23 BE03 BE21 BE23 BE32 BE33
Claims (5)
Ｋ）以上であり、かつ室温から２００℃までにおいて４
５Ｗ／（ｍ・Ｋ）以上であることを特徴とする窒化ケイ
素質焼結体。1. The thermal conductivity is 75 W / (m · m.
K) or more and 4 from room temperature to 200 ° C.
A silicon nitride-based sintered body characterized by being at least 5 W / (m · K).
物、窒化物または酸窒化物の１種以上を６ｗｔ％以下添
加して得られた窒化ケイ素質焼結体であって、相対密度
が９７％以上であり、室温において３点曲げ強度が８０
０ＭＰａ以上であることを特徴とする請求項１に記載の
窒化ケイ素質焼結体。2. A silicon nitride sintered body obtained by adding at least 6 wt% of an oxide, nitride or oxynitride as a sintering aid to silicon nitride powder, wherein the relative density is 97% or more and a three-point bending strength of 80 at room temperature.
The silicon nitride sintered body according to claim 1, wherein the sintered body is 0 MPa or more.
グネシウムおよび／または酸化イットリウムを６ｗｔ％
以下添加して得られた窒化ケイ素質焼結体であって、そ
の添加量が重量比で、酸化マグネシウム／酸化イットリ
ウム≦３．０を満足することを特徴とする請求項１また
は２に記載の窒化ケイ素質焼結体。3. A silicon nitride powder containing 6 wt% of magnesium oxide and / or yttrium oxide as a sintering aid.
The silicon nitride-based sintered body obtained by adding below, wherein the amount of addition satisfies magnesium oxide / yttrium oxide ≦ 3.0 by weight. Silicon nitride based sintered body.
とき、柱状のβ型窒化ケイ素粒子の内、長軸の長さが１
０μｍを超えるものが、１ｍｍ2当たりに２００００個
以下であることを特徴とする請求項１〜３のいずれかに
記載の窒化ケイ素質焼結体。4. When observing a cut surface of the silicon nitride based sintered body, the length of the long axis of the columnar β-type silicon nitride particles is 1
In excess of 0μm is silicon nitride sintered body according to claim 1, characterized in that 20,000 or less per 1 mm 2.
イ素質焼結体を用いたことを特徴とする絶縁基板および
回路基板。5. An insulating substrate and a circuit board using the silicon nitride sintered body according to claim 1.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001096497A JP4591738B2 (en) | 2001-03-29 | 2001-03-29 | Silicon nitride sintered body |
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| JP2002293641A true JP2002293641A (en) | 2002-10-09 |
| JP4591738B2 JP4591738B2 (en) | 2010-12-01 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2019052072A (en) * | 2017-09-19 | 2019-04-04 | 株式会社Maruwa | Silicon nitride sintered body substrate, electronic device, and method of manufacturing silicon nitride sintered body substrate |
| WO2020203683A1 (en) * | 2019-03-29 | 2020-10-08 | デンカ株式会社 | Silicon nitride sintered body, method for producing same, multilayer body and power module |
| WO2022156634A1 (en) * | 2021-01-20 | 2022-07-28 | 中国科学院上海硅酸盐研究所 | Preparation method for copper plate-covered silicon nitride ceramic substrate |
| WO2023171511A1 (en) * | 2022-03-10 | 2023-09-14 | デンカ株式会社 | Sintered ceramic object, production method therefor, and sintering-aid powder |
| WO2023171510A1 (en) * | 2022-03-10 | 2023-09-14 | デンカ株式会社 | Ceramic sintered body, method for manufacturing same, and sintering aid powder |
| JP7610660B1 (en) | 2023-08-22 | 2025-01-08 | 株式会社Maruwa | Silicon nitride sintered body, insulated circuit board, and semiconductor device |
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| JPH0930866A (en) * | 1995-07-21 | 1997-02-04 | Nissan Motor Co Ltd | High thermal conductivity silicon nitride sintered body, method for producing the same, and insulating substrate made of silicon nitride sintered body |
Cited By (12)
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|---|---|---|---|---|
| JP2019052072A (en) * | 2017-09-19 | 2019-04-04 | 株式会社Maruwa | Silicon nitride sintered body substrate, electronic device, and method of manufacturing silicon nitride sintered body substrate |
| WO2020203683A1 (en) * | 2019-03-29 | 2020-10-08 | デンカ株式会社 | Silicon nitride sintered body, method for producing same, multilayer body and power module |
| JPWO2020203683A1 (en) * | 2019-03-29 | 2020-10-08 | ||
| JP7611816B2 (en) | 2019-03-29 | 2025-01-10 | デンカ株式会社 | Method for producing sintered silicon nitride |
| WO2022156634A1 (en) * | 2021-01-20 | 2022-07-28 | 中国科学院上海硅酸盐研究所 | Preparation method for copper plate-covered silicon nitride ceramic substrate |
| US12351524B2 (en) | 2021-01-20 | 2025-07-08 | Shanghai Institute Of Ceramics, Chinese Academy Of Sciences | Preparation method for copper plate-covered silicon nitride ceramic substrate |
| WO2023171511A1 (en) * | 2022-03-10 | 2023-09-14 | デンカ株式会社 | Sintered ceramic object, production method therefor, and sintering-aid powder |
| WO2023171510A1 (en) * | 2022-03-10 | 2023-09-14 | デンカ株式会社 | Ceramic sintered body, method for manufacturing same, and sintering aid powder |
| JP7401718B1 (en) * | 2022-03-10 | 2023-12-19 | デンカ株式会社 | Silicon nitride sintered body and sintering aid powder |
| JP7408884B1 (en) * | 2022-03-10 | 2024-01-05 | デンカ株式会社 | Silicon nitride sintered body and sintering aid powder |
| JP7610660B1 (en) | 2023-08-22 | 2025-01-08 | 株式会社Maruwa | Silicon nitride sintered body, insulated circuit board, and semiconductor device |
| JP2025029631A (en) * | 2023-08-22 | 2025-03-07 | 株式会社Maruwa | Silicon nitride sintered body, insulating circuit board, and semiconductor device |
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