JP2001073048A - Aluminum-silicon carbide composite material and method for producing the same - Google Patents
Aluminum-silicon carbide composite material and method for producing the sameInfo
- Publication number
- JP2001073048A JP2001073048A JP24458499A JP24458499A JP2001073048A JP 2001073048 A JP2001073048 A JP 2001073048A JP 24458499 A JP24458499 A JP 24458499A JP 24458499 A JP24458499 A JP 24458499A JP 2001073048 A JP2001073048 A JP 2001073048A
- Authority
- JP
- Japan
- Prior art keywords
- silicon carbide
- aluminum
- composite material
- component
- sic
- 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.)
- Pending
Links
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 90
- 239000002131 composite material Substances 0.000 title claims abstract description 46
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 15
- 239000002245 particle Substances 0.000 claims abstract description 73
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 63
- 238000005245 sintering Methods 0.000 claims abstract description 33
- 239000000203 mixture Substances 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims description 49
- 239000000843 powder Substances 0.000 claims description 47
- 239000004065 semiconductor Substances 0.000 claims description 20
- 238000000465 moulding Methods 0.000 claims description 19
- 238000005242 forging Methods 0.000 claims description 14
- 229910052782 aluminium Inorganic materials 0.000 claims description 11
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 10
- 238000002844 melting Methods 0.000 claims description 10
- 230000008018 melting Effects 0.000 claims description 10
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- 238000010304 firing Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 20
- 239000002994 raw material Substances 0.000 abstract description 20
- 239000000758 substrate Substances 0.000 description 22
- 238000010438 heat treatment Methods 0.000 description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 9
- 229910000838 Al alloy Inorganic materials 0.000 description 8
- 239000012535 impurity Substances 0.000 description 8
- 229910045601 alloy Inorganic materials 0.000 description 6
- 239000000956 alloy Substances 0.000 description 6
- 238000001816 cooling Methods 0.000 description 6
- 239000013078 crystal Substances 0.000 description 6
- 239000011812 mixed powder Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- CAVCGVPGBKGDTG-UHFFFAOYSA-N alumanylidynemethyl(alumanylidynemethylalumanylidenemethylidene)alumane Chemical compound [Al]#C[Al]=C=[Al]C#[Al] CAVCGVPGBKGDTG-UHFFFAOYSA-N 0.000 description 5
- 230000017525 heat dissipation Effects 0.000 description 5
- 230000008595 infiltration Effects 0.000 description 5
- 238000001764 infiltration Methods 0.000 description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 239000011230 binding agent Substances 0.000 description 4
- 125000002091 cationic group Chemical group 0.000 description 4
- 230000007547 defect Effects 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 238000007731 hot pressing Methods 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000005266 casting Methods 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 230000001590 oxidative effect Effects 0.000 description 3
- 230000005855 radiation Effects 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 238000010306 acid treatment Methods 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 239000011362 coarse particle Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000010828 elution Methods 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 238000010406 interfacial reaction Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 230000002093 peripheral effect Effects 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- 238000009715 pressure infiltration Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 229910017980 Ag—Sn Inorganic materials 0.000 description 1
- 238000007088 Archimedes method Methods 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical group [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000011088 calibration curve Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 230000005674 electromagnetic induction Effects 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000003562 lightweight material Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000001465 metallisation Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000001272 pressureless sintering Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 229910000679 solder Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
Landscapes
- Powder Metallurgy (AREA)
Abstract
(57)【要約】
【課題】 アルミニウム−炭化珪素系複合材料の製造に
おいて、特に炭化珪素が６０体積％以上の組成域で、成
形性の向上を図り、より緻密で、より優れた熱伝導性の
同材料を得る。
【解決手段】 炭化珪素粒子の含有量が６０〜７５体積
％の組成領域内で、炭化珪素原料として、平均粒径２０
〜１７０μｍ、同粒径の標準偏差３５〜６０μｍにコン
トロールされたものを使い、この成形体を焼結すること
によって得られ、相対密度が９０％以上で１９０Ｗ／ｍ
・Ｋ以上（通常２００Ｗ／ｍ・Ｋ以上）の熱伝導率を有
するアルミニウム−炭化珪素系複合材料。
(57) Abstract: In the production of an aluminum-silicon carbide based composite material, the moldability is improved, particularly in a composition region in which silicon carbide is 60% by volume or more, and a denser and more excellent thermal conductivity is obtained. To obtain the same material. SOLUTION: In a composition region in which the content of silicon carbide particles is 60 to 75% by volume, the average particle diameter is 20 as a silicon carbide raw material.
Obtained by sintering this molded product using a material having the same particle diameter controlled to a standard deviation of 35 to 60 μm, and having a relative density of 90% or more and 190 W / m.
-An aluminum-silicon carbide composite material having a thermal conductivity of K or more (usually 200 W / mK or more).
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、各種装置・機器に
用いられる放熱基板、特に半導体装置の放熱基板に用い
られる高い熱伝導性を有するアルミニウム−炭化珪素系
複合材料およびそれを用いた半導体装置に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a heat-dissipating substrate used for various devices and equipment, and particularly to an aluminum-silicon carbide composite material having high thermal conductivity used for a heat-dissipating substrate of a semiconductor device and a semiconductor device using the same. About.
【０００２】[0002]
【従来の技術】近年半導体装置の高速演算・高集積化に
対する市場の要求は急速に高まりつつある。それととも
に、同装置の半導体素子搭載用放熱基板には、同素子か
ら発生する熱をより一層効率良く逃がすため、その熱伝
導率のより一層の向上が求められてきた。さらに同素子
ならびに同基板に隣接配置された同装置内の他の部材
(周辺部材)との間の熱歪みをより一層小さくするため
に、より一層それらに近い熱膨張係数を有するものであ
ることも求められてきた。 具体的には、半導体素子と
して通常用いられるＳｉ、ＧａＡｓの熱膨張係数がそれ
ぞれ４．２×１０-6／℃、６．５×１０-6／℃であり、
半導体装置の外囲器材として通常用いられるアルミナセ
ラミックスのそれが６．５×１０-6／℃程度であること
から、同基板の熱膨張係数はこれらの値に近いことが望
まれる。2. Description of the Related Art In recent years, market demands for high-speed operation and high integration of semiconductor devices have been rapidly increasing. At the same time, the heat radiation board for mounting the semiconductor element of the device has been required to further improve the thermal conductivity in order to more efficiently release the heat generated from the element. In addition, other members in the same device and the same device arranged adjacent to the same substrate
In order to further reduce the thermal strain between them and the (peripheral member), it is also required to have a thermal expansion coefficient closer to them. Specifically, Si usually used as the semiconductor element, the thermal expansion coefficient of GaAs are each 4.2 × 10 -6 /℃,6.5×10 -6 / ℃ ,
Since that of alumina ceramics usually used as an envelope of a semiconductor device is about 6.5 × 10 −6 / ° C., it is desired that the thermal expansion coefficient of the substrate be close to these values.
【０００３】また近年のエレクトロニクス機器の応用範
囲の著しい拡張にともない、半導体装置の使用範囲はよ
り一層多様化しつつある。このためこれらの機器に使わ
れる放熱基板は、その熱伝導率を向上させるとともに、
その熱膨張係数の周辺部材のそれとの整合性を高めるこ
とが重要である。[0003] With the remarkable expansion of the application range of electronic equipment in recent years, the range of use of semiconductor devices has been further diversified. For this reason, the heat dissipation board used in these devices improves its thermal conductivity,
It is important to enhance the matching of the coefficient of thermal expansion with that of the peripheral members.
【０００４】このような基板には、従来より例えばＣｕ
−Ｗ系やＣｕ−Ｍｏ系の複合合金からなるものが用いら
れてきた。これらの基板は、原料が高価なためにコスト
高になるとともに重量が大きくなるという問題があっ
た。そこで、最近は安価で軽量な材料として各種のアル
ミニウム(以下単にＡｌとも言う)複合合金が注目される
ようになってきた。中でもＡｌと炭化珪素(以下単にＳ
ｉＣとも言う)を主成分とするＡｌ−ＳｉＣ系複合合金
は、それらの原料が比較的安価であり、軽量かつ高熱伝
導性である。なお通常市販されている純粋なＡｌ、Ｓｉ
Ｃ単体の密度は、それぞれ２．７ｇ／ｃｍ3程度、３．
２ｇ／ｃｍ3程度、熱伝導率は、それぞれ２４０Ｗ／ｍ
・Ｋ程度、２００〜３００Ｗ／ｍ・Ｋ程度までである
が、さらにその純度や欠陥濃度を調整すれば、その熱伝
導率のレベルはさらに向上するものと思われる。そのた
め、特に注目されている材料である。また純粋なＳｉＣ
単体、Ａｌ単体の熱膨張係数はそれぞれ４．２×１０-6
／℃程度、２４×１０-6／℃程度であり、それらを複合
化することによって、その熱膨張係数が広い範囲で制御
可能となる。したがってこの点でも有利である。[0004] Conventionally, such a substrate is made of, for example, Cu.
-W-based and Cu-Mo-based composite alloys have been used. These substrates have a problem that the cost is high and the weight is large because the raw material is expensive. Therefore, recently, various aluminum (hereinafter, also simply referred to as Al) composite alloys have been attracting attention as inexpensive and lightweight materials. Among them, Al and silicon carbide (hereinafter simply referred to as S
Al-SiC-based composite alloys whose main component is iC) are relatively inexpensive, light in weight, and have high thermal conductivity. In addition, pure Al, Si which is usually
The density of C alone is about 2.7 g / cm 3 , respectively.
About 2 g / cm 3 , each having a thermal conductivity of 240 W / m 3
K, up to about 200-300 W / mK, but it is expected that the level of thermal conductivity will be further improved by further adjusting its purity and defect concentration. Therefore, it is a material that has received special attention. Also pure SiC
The thermal expansion coefficients of the simple substance and the simple substance of Al are each 4.2 × 10 −6.
/ ° C. and 24 × 10 −6 / ° C. By combining them, the thermal expansion coefficient can be controlled in a wide range. Therefore, this point is also advantageous.
【０００５】かかるＡｌ−ＳｉＣ系複合合金およびその
製造方法については、(１)特開平１−５０１４８９号公
報、(２)特開平２−２４３７２９号公報、(３)特開昭６
１−２２２６６８号公報および(４)特開平９−１５７７
７３号公報に開示されている。(１)は、ＳｉＣとＡｌの
混合物中のＡｌを溶融させて鋳造法によって固化する方
法に関するものである。 (２)、(３)は、いずれもＳｉ
Ｃ多孔体の空隙にＡｌを溶浸する方法に関するものであ
る。この内(３)は、加圧下でＡｌを溶浸する、いわゆる
加圧溶浸法に関するものである。また(４)は、ＳｉＣと
Ａｌの混合粉末の成形体かまたはそれをホットプレスし
たものを型内に配置し、これを真空中、Ａｌの融点以上
の温度で液相焼結する方法に関するものである。[0005] Such an Al-SiC-based composite alloy and its manufacturing method are described in (1) JP-A-1-501489, (2) JP-A-2-243729, and (3) JP-A-6
1-222668 and (4) JP-A-9-1577.
No. 73 is disclosed. (1) relates to a method in which Al in a mixture of SiC and Al is melted and solidified by a casting method. (2) and (3) are both Si
The present invention relates to a method of infiltrating Al into voids of a C porous body. (3) relates to a so-called pressure infiltration method in which Al is infiltrated under pressure. Also, (4) relates to a method of sintering a compact of a mixed powder of SiC and Al or a hot-pressed compact in a mold and subjecting the compact to a liquid phase sintering at a temperature equal to or higher than the melting point of Al in a vacuum. It is.
【０００６】また特開平１０−３３５５３８号公報に
は、(５)液相焼結法によって得られ、その熱伝導率が１
８０Ｗ／ｍ・Ｋ以上のアルミニウム−炭化珪素系複合材
料を提示している。この複合材料は、例えば１０〜７０
重量％の粒子状ＳｉＣ粉末とＡｌ粉末との混合粉末を成
形した後、９９％以上の窒素を含み、酸素濃度が２００
ｐｐｍ以下、露点が−２０℃以下の非酸化性雰囲気中、
６００〜７５０℃で焼結する工程によって得られる。
また特開平１０−２８００８２号公報には、(６)その熱
膨張係数が１８×１０-6／℃以下、その熱伝導率が２３
０Ｗ／ｍ・Ｋ以上であり、焼結後の寸法が実用寸法に近
い、いわゆるネットシェイプなアルミニウム−炭化珪素
系複合材料も提示している。さらに本発明者等は、特願
平１０−４１４４７号にて、(７)常圧焼結法とＨＩＰ法
とを組み合わせた同複合材料の製造方法を提案してい
る。それによれば、例えば粒子状ＳｉＣを１０〜７０重
量％混合したＡｌ−ＳｉＣ系混合粉末の成形体を、窒素
ガスを９９％以上含む非酸化性雰囲気中、６００℃以
上、Ａｌの溶融温度以下の温度範囲で常圧焼結し、熱間
鍛造するかまたはその焼結体を金属容器に封入してＨＩ
Ｐすることによって、均質でその熱伝導率が２００Ｗ／
ｍ・Ｋ以上のアルミニウム−炭化珪素系複合材料の得ら
れることを紹介した。Japanese Patent Application Laid-Open No. 10-335538 discloses that (5) a liquid phase sintering method having a thermal conductivity of 1
An aluminum-silicon carbide composite material of 80 W / m · K or more is presented. This composite material is, for example, 10-70
After forming a mixed powder of the particulate SiC powder and the Al powder in the amount of 100% by weight, it contains 99% or more of nitrogen and has an oxygen concentration of 200%.
ppm or less, in a non-oxidizing atmosphere with a dew point of -20 ° C or less,
Obtained by a process of sintering at 600 to 750 ° C.
JP-A-10-280082 discloses that (6) its thermal expansion coefficient is 18 × 10 −6 / ° C. or less and its thermal conductivity is 23.
A so-called net-shaped aluminum-silicon carbide based composite material having a size of 0 W / m · K or more and a size after sintering is close to a practical size is also proposed. Further, the present inventors have proposed in Japanese Patent Application No. 10-41447 a method (7) for producing the same composite material by combining the normal pressure sintering method and the HIP method. According to this, for example, a compact of Al-SiC-based mixed powder in which 10 to 70% by weight of particulate SiC is mixed is placed in a non-oxidizing atmosphere containing 99% or more of nitrogen gas at 600 ° C or more and a melting temperature of Al or less. Pressureless sintering in the temperature range and hot forging or sealing the sintered body in a metal container
By performing P, it is homogeneous and its thermal conductivity is 200 W /
It was introduced that an aluminum-silicon carbide composite material having a mK or more can be obtained.
【０００７】さらに(８)特開平９−１５７７７３号公報
には、（８）Ａｌ粉末とＳｉＣ粉末との混合物をホット
プレスし、成形と焼結とを同時に行う方法が開示されて
いる。その方法は、Ａｌ１０〜８０体積％、残部ＳｉＣ
の混合粉末を成形し、Ａｌの溶融点以上の温度下５００
ｋｇ／ｃｍ2以上の圧力でホットプレスするものであ
る。この方法によって１５０〜２８０Ｗ／ｍ・Ｋの熱伝
導率のアルミニウム−炭化珪素系複合材料が得られてい
る。Further, (8) Japanese Patent Application Laid-Open No. 9-157773 discloses a method of hot-pressing a mixture of (8) an Al powder and a SiC powder to simultaneously perform molding and sintering. The method is as follows: Al 10 to 80% by volume, balance SiC
And mixed powder at a temperature not lower than the melting point of Al 500
The hot pressing is performed at a pressure of kg / cm 2 or more. According to this method, an aluminum-silicon carbide composite material having a thermal conductivity of 150 to 280 W / m · K is obtained.
【０００８】[0008]
【発明が解決しようとする課題】例えば上記(８)の特開
平９−１５７７７３号公報に記載のＡｌ−ＳｉＣ系のも
のでは、その熱膨張係数を１０×１０-6／℃以下にしよ
うとすると、そのＳｉＣ量を８０体積％以上にしなけれ
ばならない。その結果１５７Ｗ／ｍ・Ｋ以下の熱伝導率
のものしか得られない。また上記(５)特開平１０−３３
５５３８号公報に記載のＡｌ−ＳｉＣ系のものでは、同
じ熱膨張係数のものを得ようとすると、そのＳｉＣ量を
６０体積％以上にしなければならない。その結果２００
Ｗ／ｍ・Ｋ程度の熱伝導率のものしか得られない。また
常圧焼結法とＨＩＰ法を組み合わせた(７)の方法で作製
されたものでも、同じ熱膨張係数のものを得ようとする
と、そのＳｉＣ量を６０重量％以上にしなければならな
い。したがって２００Ｗ／ｍ・Ｋ程度以下の熱伝導率の
ものしか得られない。For example, in the case of the Al-SiC type described in Japanese Patent Application Laid-Open No. 9-157773 described in (8) above, if the coefficient of thermal expansion is to be reduced to 10 × 10 −6 / ° C. or less. , The amount of SiC must be 80% by volume or more. As a result, only those having a thermal conductivity of 157 W / m · K or less can be obtained. Also, as described in (5) of JP-A-10-33
In the case of the Al-SiC-based material described in Japanese Patent No. 5538, in order to obtain the same thermal expansion coefficient, the SiC amount must be 60% by volume or more. As a result 200
Only those having a thermal conductivity of about W / m · K can be obtained. Further, even in the case of the one manufactured by the method (7) in which the normal pressure sintering method and the HIP method are combined, in order to obtain the same thermal expansion coefficient, the SiC amount must be 60% by weight or more. Therefore, only those having a thermal conductivity of about 200 W / m · K or less can be obtained.
【０００９】これらのＡｌ−ＳｉＣ系複合材料では、種
々の課題を抱えている。まず上記（１）に記載の製造方
法は、鋳造法であるが、ＡｌとＳｉＣの密度差により冷
却時に成形体中のＳｉＣ粒子の偏析が生じ、固化体の組
成が不均一になり易い。また上記(２)および(３)の溶浸
法では、溶浸後のＡｌの溶出部が外周に固着し、その除
去に多大の手間がかかる。上記(５)に記載された焼結法
でも軽度ではあるがこれと同じ現象が生じる。上記(６)
に記載された方法は、Ａｌの溶出を防止するため、溶浸
前のＳｉＣ多孔体の外周に薄い層を形成するものである
が、この層の溶浸後の除去には手間がかかる。また上記
(３)の加圧溶浸法では、Ａｌ未溶浸の部分(鉄鋼での引
け巣に相当する)ができ易いため、冷却時の温度勾配と
加圧・加熱のプログラムとを同時に精度良く制御できる
複雑な制御機構が必要であり、その装置はかなり高価な
ものとなる。上記（４）の型内でのホットプレスの場合
でも型外への溶融物が流出し易いため、均一組成のもの
を得ようとすると、非常に高価な製造装置が必要とな
る。These Al-SiC composite materials have various problems. First, the production method described in the above (1) is a casting method. However, due to a difference in density between Al and SiC, segregation of SiC particles in the compact occurs during cooling, and the composition of the solidified body tends to be non-uniform. In the infiltration methods (2) and (3), the elution portion of Al after infiltration adheres to the outer periphery, and it takes a lot of trouble to remove it. Although the sintering method described in the above (5) is mild, the same phenomenon occurs. The above (6)
In the method described in (1), a thin layer is formed on the outer periphery of the porous SiC body before infiltration in order to prevent the elution of Al, but removal of this layer after infiltration requires time and effort. Also above
In the pressure infiltration method (3), Al uninfiltrated portions (corresponding to shrinkage cavities in steel) are easily formed, so the temperature gradient during cooling and the pressurization / heating program are simultaneously and accurately controlled. It requires a complicated control mechanism that can be used, and the device becomes considerably expensive. Even in the case of the hot pressing in the mold of the above (4), since the melt easily flows out of the mold, an extremely expensive manufacturing apparatus is required to obtain a uniform composition.
【００１０】以上述べたように、鋳造法、溶浸法、焼結
法、ホットプレス法およびそれらを組み合わせた方法で
の品質上ならびに生産上の課題はいくつかある。これら
の方法の内で常圧下で焼結する方法は、生産性は比較的
優れているが、この方法では優れた熱伝導性のものが未
だに得られていない。一般に物質の熱伝導率は、以下の
式に示されるように物質の密度、比熱、熱拡散率の関数
である。 熱伝導率＝密度×比熱×熱拡散率 式(１) ここで複合材料の場合、比熱はその成分組成比率によっ
て決まる。したがって、組成が同じであれば、その熱伝
導率向上のためにはその密度と熱拡散率を上げることが
必要である。As described above, there are several problems in quality and production in the casting method, the infiltration method, the sintering method, the hot pressing method and the method combining them. Among these methods, the method of sintering under normal pressure has relatively high productivity, but an excellent thermal conductivity has not yet been obtained by this method. In general, the thermal conductivity of a substance is a function of the density, specific heat, and thermal diffusivity of the substance as shown in the following equation. Thermal conductivity = Density x Specific heat x Thermal diffusivity Formula (1) Here, in the case of a composite material, the specific heat is determined by the composition ratio of the components. Therefore, if the composition is the same, it is necessary to increase the density and the thermal diffusivity in order to improve the thermal conductivity.
【００１１】そこで本発明者は、特にＳｉＣ量が６０体
積％以上の焼結体の密度を上げるためには、まず成形体
の相対密度（成形体の重量をその体積で割った嵩密度
を、同じ組成の理論密度で割った値を％表示したもの）
を向上させる必要があることに着目した。その理由は以
下の通りである。前述のようにＡｌ−ＳｉＣ系複合材料
の焼結後の密度は、ＳｉＣの量によって変わるが、特に
ＳｉＣ量が６０体積％以上になると、その焼結時の収縮
が僅かになる。それ故成形体の相対密度を上げておかな
いと、常圧下の焼結では密度の向上が余り期待できない
からである。実際ＳｉＣ量が６０体積％以上になると、
この現象は顕著である。例えばＳｉＣ量が６７体積％の
成形体では、通常の乾式粉末プレスで成形された成形体
の場合、その相対密度は高々９１％程度であり、それを
焼結しても収縮率は１％以内であり、その結果得られる
材料の熱伝導率は、せいぜい１８０Ｗ／ｍ・Ｋである。In order to increase the density of a sintered body having a SiC content of 60% by volume or more, the present inventor must first determine the relative density of the molded body (the bulk density obtained by dividing the weight of the molded body by its volume, The value obtained by dividing by the theoretical density of the same composition is expressed in%)
Focused on the need to improve The reason is as follows. As described above, the density of the Al-SiC-based composite material after sintering varies depending on the amount of SiC. In particular, when the amount of SiC is 60% by volume or more, shrinkage during sintering is small. Therefore, unless the relative density of the compact is increased, the density cannot be expected to be much improved by sintering under normal pressure. Actually, when the SiC amount becomes 60% by volume or more,
This phenomenon is remarkable. For example, in the case of a compact having a SiC content of 67% by volume, the relative density of a compact formed by a normal dry powder press is at most about 91%, and even when it is sintered, the shrinkage ratio is within 1%. And the thermal conductivity of the resulting material is at most 180 W / m · K.
【００１２】[0012]
【課題を解決するための手段】したがって本発明の目的
は、ＳｉＣ量が６０体積％以上のアルミニウム−炭化珪
素系複合材料の粉末成形体を常圧焼結するか、または短
時間の熱間鍛造するかいずれかの方法によって、従来に
ない高い密度と熱伝導性を備えた焼結体を安価に提供す
ることである。すなわち本発明によって提供される複合
材料は、アルミニウムを主成分とする金属を第一成分と
し、炭化珪素粒子を第二成分とするアルミニウム−炭化
珪素系複合材料であって、この炭化珪素粒子の含有量が
６０〜７５体積％であり、同粒子の平均粒径が２０〜１
７０μｍ、同粒径の標準偏差が３５〜６０μｍであるア
ルミニウム−炭化珪素系複合材料である。この中には、
炭化珪素粒子の含有量をｘ体積％とした時、その相対密
度ｙが、（−０．２７ｘ＋１１０）％を越える複合材料
も含まれる。SUMMARY OF THE INVENTION Accordingly, an object of the present invention is to sinter a powder compact of an aluminum-silicon carbide composite material having an SiC content of 60% by volume or more under normal pressure or to perform hot forging for a short time. An object of the present invention is to provide an inexpensive sintered body having a high density and thermal conductivity that has not been achieved by the conventional method. That is, the composite material provided by the present invention is an aluminum-silicon carbide-based composite material containing aluminum as a main component as a first component and silicon carbide particles as a second component. And the average particle size of the particles is 20 to 1%.
It is an aluminum-silicon carbide composite material having a diameter of 70 μm and a standard deviation of the same particle diameter of 35 to 60 μm. In this,
Assuming that the content of silicon carbide particles is x% by volume, a composite material having a relative density y exceeding (−0.27x + 110)% is also included.
【００１３】本発明の複合材料は、平均粒径が２０〜１
７０μｍ、同粒径の標準偏差が３５〜６０μｍである炭
化珪素粒子からなる上記第二成分の粉末６０〜７５体積
％と、上記第一成分の粉末３５〜４０体積％とを混合し
混合物とする工程と、同混合物を成形し成形体とする工
程と、同成形体を第一成分の融点以上の温度で焼結し焼
結体とする工程とを含む製造方法によって得られる。こ
の方法の中には、この成形体とする工程において、成形
圧力が４ｔｏｎ／ｃｍ2以上であり、炭化珪素粒子の含
有量をｘ体積％とした時、得られる成形体の相対密度ｙ
を（−０．２７ｘ＋１１０）％以上とする方法が含まれ
る。この成形体は、焼結によって少なくともこれを越え
るレベルの相対密度となる。またこの焼結体とする工程
が、熱間鍛造によって行われる方法も含まれる。The composite material of the present invention has an average particle size of 20 to 1
70 to 75% by volume of the second component powder composed of silicon carbide particles having a particle diameter of 70 to 70 μm and a standard deviation of 35 to 60 μm, and 35 to 40% by volume of the first component powder to form a mixture. It is obtained by a manufacturing method including a step, a step of molding the mixture to form a molded body, and a step of sintering the molded body at a temperature equal to or higher than the melting point of the first component to form a sintered body. In this method, when the molding pressure is 4 ton / cm 2 or more and the content of silicon carbide particles is x volume% in the step of forming the molded body, the relative density y of the obtained molded body is determined.
Is set to (−0.27x + 110)% or more. The compact has a relative density of at least a level higher than the above by sintering. In addition, a method in which the step of forming the sintered body is performed by hot forging is also included.
【００１４】さらに本発明には、以上の複合材料を用い
た半導体装置も含まれる。The present invention further includes a semiconductor device using the above composite material.
【００１５】[0015]
【発明の実施の形態】本発明の複合材料は、前記のよう
に第二成分の炭化珪素を主成分とする粒子を６０〜７５
体積％含み、この第二成分の粒子の粒度分布をコントロ
ールしたものである。すなわち本発明の複合材料の第二
成分粒子は、微粒と粗粒とを適正な比率で含む形態で存
在する。具体的には、平均粒径が２０〜１７０μｍの範
囲内にあり、同粒径の標準偏差が３５〜６０μｍとなる
ようにコントロールする。好ましくは平均粒径および粒
径の標準偏差がそれぞれ４０〜１３０μｍおよび４０〜
５０μｍである。平均粒径および粒径の標準偏差が上記
範囲を外れると、いずれも相対密度が９０％未満とな
り、その結果熱伝導率が１９０Ｗ／ｍ・Ｋ未満に低下す
る。BEST MODE FOR CARRYING OUT THE INVENTION As described above, the composite material of the present invention contains 60 to 75 particles containing silicon carbide as the main component as the second component.
%, And controls the particle size distribution of the particles of the second component. That is, the second component particles of the composite material of the present invention exist in a form containing fine particles and coarse particles at an appropriate ratio. Specifically, control is performed so that the average particle size is in the range of 20 to 170 μm, and the standard deviation of the same particle size is 35 to 60 μm. Preferably, the average particle size and the standard deviation of the particle size are 40 to 130 μm and 40 to 130 μm, respectively.
50 μm. When the average particle diameter and the standard deviation of the particle diameter are out of the above ranges, the relative density becomes less than 90% and the thermal conductivity is reduced to less than 190 W / m · K.
【００１６】また本発明の複合材料には、炭化珪素粒子
の含有量をｘ体積％とした時、その相対密度ｙが、（−
０．２７ｘ＋１１０）％を越えるものも含まれる。炭化
珪素粒子の量と相対密度の関係をこのようにすると、熱
伝導率２００Ｗ／ｍ・Ｋ以上の優れた熱伝導性の材料が
得られる。In the composite material of the present invention, when the content of silicon carbide particles is x volume%, the relative density y is (−).
0.27x + 110)%. By setting the relationship between the amount of silicon carbide particles and the relative density in this way, a material having excellent thermal conductivity of 200 W / m · K or more in thermal conductivity can be obtained.
【００１７】本発明の複合材料は、前記の方法によって
得られる。原料となる第一成分・第二成分の粉末は、市
販のものでよいが、できるだけ純度の高いものであるの
が望ましい。特に第二成分のＳｉＣ粉末は、本質的に熱
伝導性に優れた６Ｈ型や４Ｈ型のような結晶型のもので
あるのが好ましい。また陽イオン不純物（遷移金属元
素）、特に鉄族元素の含有量、積層欠陥、点欠陥、結晶
歪みおよび転移のような欠陥の量が少なく、さらにはキ
ャリヤ濃度の小さな粒子からなる粉末を選ぶのが望まし
い。陽イオン不純物の量は、１００ｐｐｍ以下にするの
が望ましい。市販の上記結晶型の粒子からなる粉末を使
い、予め加熱処理および／または酸処理を行って欠陥や
不純物の量を減らしてもよい。熱処理は、例えば不活性
ガス雰囲気中、１６００〜２４００℃の温度範囲で行
う。また酸処理は、例えばフッ酸、硝酸、塩酸のような
酸の水溶液に浸漬する。またＳｉＣ粉末の熱伝導率を高
めるには、上記した陽イオン不純物の他にＮの結晶中へ
の固溶量を減らす必要がある。用いるＳｉＣ粉末のキャ
リヤ濃度は、低いほどよいが、特に５×１０19／ｃｍ3
以下とするのが望ましい。The composite material of the present invention is obtained by the above method. The powders of the first and second components used as raw materials may be commercially available, but are desirably as pure as possible. In particular, the SiC powder of the second component is preferably of a crystal type such as a 6H type or a 4H type which is essentially excellent in thermal conductivity. Also, select powders that consist of particles with low content of cationic impurities (transition metal elements), especially the content of iron group elements, stacking faults, point defects, crystal distortion and dislocation, and low carrier concentration. Is desirable. It is desirable that the amount of the cationic impurities be 100 ppm or less. The amount of defects and impurities may be reduced by performing a heat treatment and / or an acid treatment in advance using a commercially available powder composed of the above-mentioned crystal-type particles. The heat treatment is performed, for example, in an inert gas atmosphere in a temperature range of 1600 to 2400 ° C. In the acid treatment, the substrate is immersed in an aqueous solution of an acid such as hydrofluoric acid, nitric acid or hydrochloric acid. Further, in order to increase the thermal conductivity of the SiC powder, it is necessary to reduce the amount of N dissolved in the crystal in addition to the above-mentioned cationic impurities. The lower the carrier concentration of the SiC powder to be used, the better, but especially 5 × 10 19 / cm 3
It is desirable to do the following.
【００１８】なお使用する第二成分ＳｉＣ粉末の平均粒
径および同粒径の標準偏差は、前述のような範囲にコン
トロールする。両者をこの範囲内にすることによって、
製造面では、成形性を損ねることなく前述のように高密
度かつ高熱伝導率の材料を得ることができる。なお成形
時には、両者の範囲が下限未満では相対密度９０％以上
の成形体が得られず、一方上限を越えると成形体に亀裂
が生じるようになるので好ましくない。The average particle size of the second component SiC powder used and the standard deviation of the particle size are controlled in the above-mentioned ranges. By keeping both within this range,
In terms of manufacturing, it is possible to obtain a material having high density and high thermal conductivity as described above without impairing the formability. In the case of molding, if the range of both is less than the lower limit, a molded article having a relative density of 90% or more cannot be obtained, while if it exceeds the upper limit, cracks are formed in the molded article, which is not preferable.
【００１９】アルミニウムを主成分とする第一成分の原
料は、市販のものを用いればよい。ただし作製された複
合材料の熱伝導率を下げないためには、その純度は高い
方が望ましい。例えば９９％以上のものを用いるのが望
ましい。なお本発明で用いる第一成分の原料の使用形態
は、塊状・粉末状他のいかなる形態であってもよいが、
通常は粉末状のものを用いる。原料粉末内に介在する不
純物種としては、特にアルミニウムに固溶し易い遷移金
属元素、特に８ａ族元素を含む成分を含む成分は、可能
な限り少ないのが望ましい。したがって、市販のアルミ
ニウム合金粉末を用いる場合には、これらの合金を作る
ための成分の少ないものを選ぶのが望ましい。なおさら
にアルミニウムまたはアルミニウム合金の原料粉末のア
ルミニウム純度を高めるためには、市販の粉末の純度を
上げるため、同粉末を溶湯噴霧法、物理的または化学的
な処理法によって調製された粉末を準備する必要があ
る。なおこの第一成分粒子の粒度分布については、特に
制約は無い。The raw material of the first component containing aluminum as a main component may be a commercially available one. However, in order not to lower the thermal conductivity of the produced composite material, it is desirable that its purity is higher. For example, it is desirable to use 99% or more. In addition, the use form of the raw material of the first component used in the present invention may be any form such as a lump or powder,
Usually, a powdery one is used. As the impurity species interposed in the raw material powder, it is desirable that a component containing a transition metal element which is particularly easily dissolved in aluminum, particularly a component containing a group 8a element, is as small as possible. Therefore, when a commercially available aluminum alloy powder is used, it is desirable to select one having a small component for producing these alloys. In order to further increase the aluminum purity of the raw material powder of aluminum or aluminum alloy, in order to increase the purity of a commercially available powder, prepare a powder prepared by melting the powder, a physical or chemical treatment method, or the like. There is a need. There is no particular limitation on the particle size distribution of the first component particles.
【００２０】以上述べたように、本発明で使用する原料
は、第二成分のＳｉＣ粉末として可能な限り高純度かつ
低欠陥のものを用い、第一成分のアルミニウムを主成分
とする原料も高純度のものを用いるのが望ましい。原料
粉末は、第一成分の量が３５〜４０体積％、第二成分の
量が６０〜７５体積％となるように、秤量し混合する。
原料の混合方法は、原料の形態・性状に合わせ原料純度
が低下しない方法であれば、既存の方法でよい。また混
合物は、その成形性を高めるために、例えば顆粒状に造
粒してその嵩を下げるのが好ましい。As described above, as the raw material used in the present invention, a SiC powder of the second component having a purity and a defect as low as possible is used. It is desirable to use one of purity. The raw material powder is weighed and mixed such that the amount of the first component is 35 to 40% by volume and the amount of the second component is 60 to 75% by volume.
The method of mixing the raw materials may be an existing method as long as the raw material purity does not decrease according to the form and properties of the raw materials. Further, in order to enhance the formability of the mixture, it is preferable to reduce the bulk by, for example, granulating the mixture into granules.
【００２１】混合物の成形法については、通常のいかな
る方法であってもよい。乾式粉末成形の場合の圧力は、
４ｔｏｎ／ｃｍ2以上とするのが好ましい。この圧力設
定にすることによって、成形体中のＳｉＣ粒子の量をｘ
体積％とした時の成形体の相対密度を、（−０．２７ｘ
＋１１０）％以上にコントロールすることができる。こ
の圧力未満では成形時に第一成分粒子の表面を覆ってい
るアルミニウムの酸化物（通常はアルミナ）の被膜の破
れない確率が高くなり、成形時の両成分の密着面積が低
下し易くなる。その結果最終的に得られる複合材料の密
度や熱伝導率の固体内のばらつきが大きくなり易くな
る。より好ましくは、６ｔｏｎ／ｃｍ2以上である。The method for molding the mixture may be any conventional method. The pressure for dry powder molding is
It is preferably at least 4 ton / cm 2 . With this pressure setting, the amount of SiC particles in the compact is reduced by x
The relative density of the molded body when expressed as volume% is (−0.27 ×
+110)% or more. If the pressure is less than this, the probability that the coating of the aluminum oxide (usually alumina) covering the surface of the first component particles will not break during molding increases, and the adhesion area of both components during molding tends to decrease. As a result, variations in the density and thermal conductivity of the finally obtained composite material in the solid tend to increase. More preferably, it is 6 ton / cm 2 or more.
【００２２】なお本発明の成形工程において、従来より
も高い相対密度の成形体が得られるのは、以下のように
考えられる。Ａｌ−ＳｉＣ系の混合粉末を成形する場
合、ヤング率の高いＳｉＣ粒子は、ほとんど変形しない
が、加圧によってＡｌ粒子は、塑性変形し易いため、Ｓ
ｉＣ粒子間の隙間に侵入して行く。本発明者は、その際
のＡｌ粒子の侵入の度合が、ＳｉＣ粒子の粒度分布に強
く依存することを見出した。すなわち本発明の複合材料
の第二成分粒子は、微粒と粗粒とを上記の具体的な範囲
となるように、予め粒度調整されている。このため従来
から使われてきた粒度分布幅の狭いＳｉＣ粒子群からな
る粉末に比べ、混合粉末として成形時の圧縮性に極めて
優れている。In the molding step of the present invention, the reason why a molded article having a higher relative density than the conventional one is obtained is considered as follows. When molding an Al-SiC mixed powder, SiC particles having a high Young's modulus hardly deform, but Al particles are easily plastically deformed by pressurization.
It penetrates into the gap between iC particles. The present inventor has found that the degree of penetration of Al particles at that time strongly depends on the particle size distribution of SiC particles. That is, the particle size of the second component particles of the composite material of the present invention is adjusted in advance so that the fine particles and the coarse particles are in the above specific ranges. For this reason, compared with the powders comprising SiC particles having a narrow particle size distribution width conventionally used, the mixed powders are extremely excellent in compressibility during molding.
【００２３】成形体は、第一成分の融点以上の温度下で
加熱して常圧焼結するか、または熱間鍛造する。常圧焼
結の場合は、非酸化性雰囲気中で、通常数時間までの時
間内で行う。この焼結によってほとんど収縮しない場合
もあるが、通常はさらに収縮して、相対密度は上昇す
る。例えば前述のように、乾式成形によって４ｔｏｎ／
ｃｍ2以上の圧力で成形した成形体は、ＳｉＣ粒子の量
をｘ体積％とすると、（−０．２７ｘ＋１１０）％を越
える相対密度となる。The compact is heated at a temperature equal to or higher than the melting point of the first component and sintered under normal pressure or hot forged. In the case of normal pressure sintering, the sintering is usually performed in a non-oxidizing atmosphere within a time period of up to several hours. In some cases, this sintering hardly shrinks, but usually shrinks further and the relative density increases. For example, as described above, 4 ton /
A molded article molded at a pressure of 2 cm 2 or more has a relative density exceeding (−0.27x + 110)%, where x is the volume of SiC particles.
【００２４】また熱間鍛造は、成形体を予め第一成分の
融点以上の温度で、短時間（数分以内であり、通常は１
０秒以内）の予備的な加熱の後、予め２００℃以上に予
熱された型内で熱間鍛造する。なおこの予備加熱の時間
が数秒以内の短時間であれば、空気中で行ってもさほど
の問題はない。しかし通常の加熱方式で均一に加熱する
ためには、１０数分必要であるので、この場合には窒素
やアルゴン等の不活性ガス雰囲気が好ましい。このよう
な短時間の加熱を行う場合には、加熱方式として、例え
ばプラズマ加熱方式、電磁誘導加熱方式、マイクロ波加
熱方式のような方式を選ぶ。この種の加熱方式を採るこ
とによって、成形体内部から均一にかつ急速に加熱され
るため、目的とする温度で少なくとも数秒程度保持する
だけで、本発明の目的とする高い熱伝導性の複合材料が
得られる。このように短時間の加熱で焼結することによ
って、両主成分間の熱伝導率の低い反応生成物の生成
（例えば炭化アルミニウムすなわちＡｌ4Ｃ3の生成や両
成分に含まれる不純物と主成分との界面反応生成物の生
成）、主成分中に含まれる不純物の主成分結晶格子中へ
の固溶現象等が、かなり回避できるからである。なお鍛
造に用いる金型の予熱温度は、６００℃を越えると金型
の強度が低下することもあるので、２００〜５００℃程
度とするのが最も望ましい。この鍛造によって得られる
材料は、成形時以上に高い密度（特に成形体の相対密度
が９０％以上であれば、通常１００％）となる。なおこ
の緻密化を促進するためには、鍛造圧力は、１ｔｏｎ／
ｃｍ2以上とするのが望ましい。このようにＳｉＣ量が
ｘ体積％の時の成形体の相対密度ｙが（−０．２７ｘ＋
１１０）％を越えるように以上にコントロールするとと
もに、熱間鍛造で焼結することにより、２４０Ｗ／ｍ・
Ｋ以上の高い熱伝導率の焼結体が安定して得られる。In hot forging, a compact is preliminarily heated at a temperature equal to or higher than the melting point of the first component for a short time (within several minutes, usually 1 minute).
After preliminary heating (within 0 seconds), hot forging is performed in a mold preheated to 200 ° C. or higher in advance. If the preheating time is as short as several seconds or less, there is no significant problem even if the preheating is performed in air. However, it takes 10 minutes or more to uniformly heat by a normal heating method. In this case, an inert gas atmosphere such as nitrogen or argon is preferable. When heating in such a short time, a method such as a plasma heating method, an electromagnetic induction heating method, or a microwave heating method is selected as the heating method. By adopting this kind of heating method, the molded body is uniformly and rapidly heated from the inside, so that the composite material having high heat conductivity which is the object of the present invention can be maintained at the target temperature for at least about several seconds. Is obtained. By sintering by heating for a short time in this way, the formation of a reaction product having low thermal conductivity between the two main components (for example, the formation of aluminum carbide, ie, Al 4 C 3 , and the impurities contained in both components and the main component) This is because formation of an interfacial reaction product with) and the solid solution of impurities contained in the main component into the main component crystal lattice can be considerably avoided. If the preheating temperature of the mold used for forging exceeds 600 ° C., the strength of the mold may decrease. Therefore, it is most preferable that the preheating temperature be about 200 to 500 ° C. The material obtained by this forging has a higher density than that at the time of molding (particularly 100% if the relative density of the molded body is 90% or more). In order to promote the densification, the forging pressure should be 1 ton /
cm 2 or more is desirable. Thus, when the SiC amount is x volume%, the relative density y of the compact is (−0.27x +
110)%, and by sintering by hot forging, 240 W / m.
A sintered body having a high thermal conductivity of K or more can be stably obtained.
【００２５】本発明の複合材料は、以上述べたように緻
密かつ優れた熱伝導性を有するため半導体装置に用いら
れる各種部材、特に半導体素子の周囲に用いられる放熱
基板材料として有用である。また焼結による収縮が小さ
いため、ネットシェイプで加工に手間のかからない安価
なものや、大型で複雑な形状の部材としても有用であ
る。特に熱伝導率が２００Ｗ／ｍ・Ｋ以上のものは、電
気自動車等の輸送機器や工作機械等のパワー制御部に用
いられるパワーモジュール用の半導体装置にも有用であ
る。As described above, the composite material of the present invention is dense and has excellent thermal conductivity, and thus is useful as a material for various members used in a semiconductor device, in particular, a heat radiation substrate material used around a semiconductor element. Further, since the shrinkage due to sintering is small, it is also useful as a net-shaped, inexpensive material that does not require processing, or a large-sized member having a complicated shape. In particular, those having a thermal conductivity of 200 W / m · K or more are also useful as semiconductor devices for power modules used in power control units of transport equipment such as electric vehicles and machine tools.
【００２６】[0026]
【実施例】実施例１ 純度が９９％以上、平均粒径が１０〜１６０μｍのアル
ミニウム（Ａｌ）粉末と、陽イオン不純物の含有量が１
００ｐｐｍ以下、平均粒径が１８〜１７５μｍで粒径の
標準偏差が１０〜６２μｍ、結晶型が６Ｈ型の炭化珪素
（ＳｉＣ）粉末とを準備した。このＡｌ粉末の融点は６
５９℃であった。これらの原料粉末の中から、各試料毎
に表１の「原料平均粒径」欄に記載の平均粒径のＡｌお
よびＳｉＣの原料粉末を選び、各試料の原料の組合せに
て、同表の「組成」欄に記載の体積部のＳｉＣ量で、残
体積部がＡｌとなるように秤量した。なお「原料」欄の
括弧内の数値は、ＳｉＣ粉末の粒径の標準偏差値であ
る。その後粉末１００重量部に対し３重量部のパラフィ
ンを有機バインダーとして添加し、両原料粉末とともに
エタノール中でボールミル混合し、得られたスラリーを
噴霧乾燥して、顆粒状の造粒粉末とした。EXAMPLE 1 Aluminum (Al) powder having a purity of 99% or more and an average particle diameter of 10 to 160 μm, and a content of cationic impurities of 1
A silicon carbide (SiC) powder having a crystal form of 6H type, having a mean particle size of 18 to 175 μm, a standard deviation of the particle size of 10 to 62 μm, and a crystal form of not more than 00 ppm. The melting point of this Al powder is 6
It was 59 ° C. From these raw material powders, Al and SiC raw material powders having an average particle size described in the column of “raw material average particle size” in Table 1 were selected for each sample, and the combination of the raw materials of each sample was used. Based on the amount of SiC in the volume part described in the column of “Composition”, it was weighed so that the remaining volume part was Al. The numerical values in parentheses in the “raw material” column are standard deviation values of the particle diameter of the SiC powder. Thereafter, 3 parts by weight of paraffin was added as an organic binder to 100 parts by weight of the powder, mixed with a ball mill in ethanol together with both raw material powders, and the obtained slurry was spray-dried to obtain a granulated powder.
【００２７】その後表１に記載の各試料毎の成形圧力
で、直径が１００ｍｍ、厚みが２０ｍｍの形状の成形体
を作製した。成形体の見かけ密度（その重量を体積で割
った値）と理論密度（組成から割り出した１００％緻密
化した場合の密度）からその相対密度（見かけ密度の理
論密度に対する割合）を算定した。これらの成形体を窒
素気流中、４００℃でバインダーを除去した後、温度６
６０℃で２時間焼結した。各焼結体から適宜試験片を切
り出し、レーザーフラッシュ法によって熱伝導率を、差
動トランス方式の測定法によって熱膨張係数を、アルキ
メデス法（水中法）によって密度をそれぞれ確認した。
またこの実測した密度と理論密度とから相対密度（実測
した密度の理論密度に対する割合）を算定した。これら
の結果を表１に示す。なお焼結体中のＳｉＣおよびＡｌ
の量は、化学分析の結果ほぼ当初の混合量と同じであっ
た。またＸ線回折によって炭化アルミニウムの生成量を
確認（各試料の同化合物のメインピークとＡｌのメイン
ピークのピーク高さの比から、予め作成した同比の検量
線を用いて確認）したところ、いずれの試料も５体積％
以下であった。Thereafter, a molded body having a diameter of 100 mm and a thickness of 20 mm was produced at the molding pressure for each sample shown in Table 1. The relative density (the ratio of the apparent density to the theoretical density) was calculated from the apparent density (the value obtained by dividing the weight by the volume) and the theoretical density (the density obtained when the molded article was densified by 100%). After removing the binder from these molded bodies at 400 ° C. in a nitrogen stream, a temperature of 6 ° C.
Sintered at 60 ° C. for 2 hours. Test pieces were cut out from each sintered body as appropriate, and the thermal conductivity was confirmed by a laser flash method, the thermal expansion coefficient was measured by a differential transformer method, and the density was confirmed by an Archimedes method (underwater method).
The relative density (the ratio of the actually measured density to the theoretical density) was calculated from the actually measured density and the theoretical density. Table 1 shows the results. Note that SiC and Al in the sintered body
Was almost the same as the initially mixed amount as a result of chemical analysis. The amount of aluminum carbide generated was confirmed by X-ray diffraction (confirmed from the ratio of the peak height of the main peak of the same compound to the main peak of Al in each sample using a calibration curve of the same ratio prepared in advance). 5% by volume
It was below.
【００２８】[0028]
【表１】 [Table 1]
【００２９】以上の結果より以下のことが分かる。
（１）ＳｉＣの量が６０〜７５体積％の範囲内の組成域
において、ＳｉＣ原料粉末の粒度を、平均粒径が３５〜
１７０μｍ、粒径の標準偏差が１０〜６０μｍの範囲内
にコントロールすると、その範囲外の粒度の場合に比
べ、成形体の圧縮性が改善される。このため成形体の相
対密度が顕著に高められる。その結果常圧焼結によって
も、相対密度が９０％以上で、熱伝導率が１９０Ｗ／ｍ
・Ｋ以上の本発明材料が得られる。また（２）ＳｉＣの
量がｘ体積％の時に成形圧力を４ｔｏｎ／ｃｍ2以上と
し、その相対密度ｙを（−０．２７ｘ＋１１０）％以上
とすることによって、熱伝導率が２００Ｗ／ｍ・Ｋ以上
の材料が得られる。The following results can be understood from the above results.
(1) In the composition range where the amount of SiC is in the range of 60 to 75% by volume, the particle size of the SiC raw material powder is set to an average particle size of 35 to
When the standard deviation of the particle size is controlled within the range of 170 μm and 10 to 60 μm, the compressibility of the molded body is improved as compared with the case of the particle size outside the range. For this reason, the relative density of the compact is significantly increased. As a result, even under normal pressure sintering, the relative density is 90% or more and the thermal conductivity is 190 W / m.
-The material of the present invention of K or more is obtained. (2) By setting the molding pressure to 4 ton / cm 2 or more and the relative density y to (−0.27x + 110)% or more when the amount of SiC is x volume%, the thermal conductivity is 200 W / m · K. The above materials are obtained.
【００３０】実施例２ 実施例１と同じ調製条件で得られた表１の試料１〜１７
の各成形体を、実施例１と同じ条件でバインダーを除い
た後、高周波誘導加熱炉内に配置して、窒素中６６０℃
で表２の時間予備加熱した後、予め表２の温度に加熱し
たダイス鋼製の型に入れて、直ちに表２の圧力で熱間鍛
造した。鍛造後の試料は、実施例１と同様にして評価
し、その結果を表２に示す。なお同表記載の用いた成形
体の番号は、表１の番号に対応する。なお実施例１同様
炭化アルミニウムの生成量を確認したところ、各試料と
も同じ成形体を用いた実施例１の対応試料に比べ、全て
の試料で１／２以下であった。Example 2 Samples 1 to 17 of Table 1 obtained under the same preparation conditions as in Example 1
After removing the binder under the same conditions as in Example 1, each of the molded articles was placed in a high-frequency induction heating furnace, and was placed in nitrogen at 660 ° C.
After preheating for the time shown in Table 2, the steel was placed in a die steel mold preheated to the temperature shown in Table 2 and immediately hot forged at the pressure shown in Table 2. The sample after forging was evaluated in the same manner as in Example 1, and the results are shown in Table 2. The numbers of the molded bodies used in the table correspond to the numbers in Table 1. The amount of aluminum carbide generated was confirmed in the same manner as in Example 1. As a result, the amount of each sample was less than or equal to で in all samples as compared with the corresponding sample in Example 1 using the same compact.
【００３１】[0031]
【表２】 [Table 2]
【００３２】以上の結果より、ＳｉＣの量が６０〜７５
体積％の範囲内の組成域において、その平均粒径および
粒径の標準偏差を本発明範囲内にコントロールし、さら
に熱間鍛造によって常圧焼結（実施例１）に比べ、短時
間の緻密化が可能になることが分かる。その結果同じ成
形体でも、より優れた熱伝導性の（２４０Ｗ／ｍ・Ｋ以
上）本発明材料が得られる。常圧焼結よりも熱伝導性が
向上する主な理由は、両主成分間の界面反応による炭化
アルミニウム等の低熱伝導性化合物の生成が抑えられる
ことである。From the above results, it can be seen that the amount of SiC is 60-75.
In the composition range within the range of volume%, the average particle diameter and the standard deviation of the particle diameter are controlled within the range of the present invention. It can be seen that conversion becomes possible. As a result, even with the same molded body, the material of the present invention having more excellent thermal conductivity (240 W / m · K or more) can be obtained. The main reason why the thermal conductivity is improved as compared with the normal pressure sintering is that the generation of a low thermal conductive compound such as aluminum carbide due to an interfacial reaction between both main components is suppressed.
【００３３】実施例３ 実施例１の試料１と４で用いた二種のＳｉＣ粉末と、純
度９９％以上で平均粒径が５０μｍであり、合金成分と
して１０重量％のＳｉと４重量％のＭｇを含むＡｌ合金
の粉末とを準備した。このＡｌ合金の融点は、５９０℃
であった。まず実施例１の試料１と同じ体積部のＳｉＣ
粉末、残部が上記Ａｌ合金粉末となるように、実施例１
と同様に混合し、噴霧乾燥して顆粒状の造粒粉末を調製
した。また別途試料４と同じ体積部のＳｉＣ粉末、残部
が上記Ａｌ合金粉末となるように、実施例１と同様に混
合し、噴霧乾燥して顆粒状の造粒粉末を調製した。次い
でこれらの粉末を、それぞれ試料１および４と同じ条件
で同じ形状の成形体を作製した。成形後の相対密度は、
前者が８６％、後者が８９％であった。これらの成形体
を実施例１と同じ条件でバインダー除去した。得られた
成形体をまず実施例１と同じ常圧焼結炉内に配置し、６
００℃で２時間加熱して焼結した。Example 3 The two kinds of SiC powders used in samples 1 and 4 of Example 1 had a purity of 99% or more, an average particle size of 50 μm, and 10% by weight of Si and 4% by weight of alloy components. And an Al alloy powder containing Mg. The melting point of this Al alloy is 590 ° C
Met. First, the same volume of SiC as sample 1 of Example 1 was used.
Example 1 so that the powder and the remainder would be the Al alloy powder
And then spray-dried to prepare a granulated powder. Separately, the same volume parts as in Sample 4 were mixed and the remainder was the Al alloy powder, and the mixture was mixed and spray dried in the same manner as in Example 1 to prepare a granular granulated powder. Next, a compact having the same shape was produced from these powders under the same conditions as in Samples 1 and 4, respectively. The relative density after molding is
The former was 86% and the latter 89%. The binder was removed from these molded articles under the same conditions as in Example 1. The obtained compact was first placed in the same atmospheric sintering furnace as in Example 1,
Sintering was performed by heating at 00 ° C. for 2 hours.
【００３４】また別途これらの成形体を実施例２と同じ
高周波誘導加熱炉内に配置し、６００℃で１分間予備加
熱し、次いで実施例２の試料２８と同じ条件にて熱間鍛
造した。常圧焼結した実施例１の試料１に対応する試料
５２および同試料４に対応する試料５３と、熱間鍛造し
た実施例２の試料２５に対応する試料５４および同試料
２９に対応する試料５５を実施例１と同様に評価し、そ
の結果を表３に示す。なお炭化アルミニウムの生成量
は、試料５２と５３では５体積％以下、試料５４と５５
ではそれらの１／２以下であった。この結果より、Ａｌ
に代えてＡｌ合金を用いても、熱伝導性は低下するが、
ＳｉＣ粉末の粒度をコントロールすることによる本発明
の効果ならびに熱間鍛造による（常圧焼結えお行う場合
に対する）効果は、同じ傾向にあることが分かる。These compacts were separately placed in the same high-frequency induction heating furnace as in Example 2, pre-heated at 600 ° C. for 1 minute, and then hot forged under the same conditions as Sample 28 of Example 2. Sample 52 corresponding to Sample 1 of Example 1 and Sample 53 corresponding to Sample 4 subjected to normal pressure sintering, and Sample 54 corresponding to Sample 25 and Sample 29 corresponding to hot forged Sample 25 of Example 2 55 was evaluated in the same manner as in Example 1, and the results are shown in Table 3. The amount of aluminum carbide produced was 5% by volume or less for samples 52 and 53, and
Was less than 1/2 of those. From this result, Al
When using an Al alloy instead of, the thermal conductivity is reduced,
It can be seen that the effect of the present invention by controlling the particle size of the SiC powder and the effect of hot forging (relative to the case of performing normal pressure sintering) have the same tendency.
【００３５】[0035]
【表３】 [Table 3]
【００３６】実施例４ 表１の試料４、１１および１６、表２の試料２８、４５
および５０、表３の試料５５と同じ製造方法で作製した
放熱基板を用いた図１に示すようなパワーモジュール半
導体装置を作製した。同図において１は、本発明の材料
からなる放熱基板、２は、同基板上にロウ付けされた電
気絶縁性の窒化アルミニウムセラミックス（熱伝導率１
７０Ｗ／ｍ・Ｋ）製の小基板、３は、シリコン半導体素
子、４は、放熱基板に機械的に固定されたアルミニウム
合金からなる冷却構造体である。なお基板１の上下面と
基板１４の下面にはニッケルメッキが、基板２の上面に
はＷメタライズ層およびニッケルメッキ層を介して銅の
導体回路層が形成されている。また基板１と冷却構造体
４との界面には予めシリコーンオイルの薄い層が形成さ
れている。半導体素子はＡｇ−Ｓｎ系の半田で接続され
ている。なお各部材間、特に基板１の周辺の接続状態
は、良好で問題は無かった。また本発明の材料からなる
放熱基板１の仕上げ加工は、焼結後の材料の寸法がほぼ
ネットシェイプであったため、ブラスト加工程度の仕上
げで行うことができた。Example 4 Samples 4, 11 and 16 in Table 1 and Samples 28 and 45 in Table 2
1 and a power module semiconductor device as shown in FIG. 1 using a heat radiating substrate manufactured by the same manufacturing method as the sample 55 in Table 3. In the figure, reference numeral 1 denotes a heat dissipation substrate made of the material of the present invention, and 2 denotes an electrically insulating aluminum nitride ceramic (having a thermal conductivity of 1) brazed on the substrate.
A small substrate made of 70 W / m · K), 3 is a silicon semiconductor element, and 4 is a cooling structure made of an aluminum alloy mechanically fixed to a heat dissipation substrate. The upper and lower surfaces of the substrate 1 and the lower surface of the substrate 14 are formed with nickel plating, and the upper surface of the substrate 2 is formed with a copper conductor circuit layer via a W metallization layer and a nickel plating layer. At the interface between the substrate 1 and the cooling structure 4, a thin layer of silicone oil is formed in advance. The semiconductor elements are connected by Ag-Sn based solder. The connection between the members, especially around the periphery of the substrate 1, was good and there was no problem. Further, the finish processing of the heat radiation substrate 1 made of the material of the present invention could be performed with a finish of about blast processing because the dimensions of the material after sintering were almost net-shaped.
【００３７】このような構成の各アッセンブリーを用い
て、−６０℃で３０分間保持後、１５０℃で３０分間保
持する昇降温の冷熱サイクルを１０００サイクル行った
ところ、接続部周辺の損傷およびモジュール特性の劣化
は観測されなかった。以上の結果から本発明の方法で製
造された複合材料を、過酷な実用条件下で使われる半導
体装置の部材に用いても、何ら支障無く使用可能なこと
が判明した。Using each assembly having such a configuration, 1000 cycles of heating / cooling cycles of holding at -60 ° C. for 30 minutes and then holding at 150 ° C. for 30 minutes were performed. No deterioration was observed. From the above results, it has been found that the composite material manufactured by the method of the present invention can be used without any problem even when used for a member of a semiconductor device used under severe practical conditions.
【００３８】なお本発明の材料をこの種のモジュールに
比べ低出力・低熱負荷のパーソナルコンピュータ等の半
導体装置に実装する評価も行ったが、その実用信頼性に
は何ら問題の無いことが確認された。It was also evaluated that the material of the present invention is mounted on a semiconductor device such as a personal computer having a lower output and a lower heat load than this type of module, but it has been confirmed that there is no problem in its practical reliability. Was.
【００３９】[0039]
【発明の効果】以上述べてきたように本発明によれば、
アルミニウムを主成分とする金属を第一成分とし、炭化
珪素粒子を第二成分とするアルミニウム−炭化珪素系複
合材料の製造方法において、炭化珪素粒子の含有量が６
０〜７５体積％の組成領域内で、炭化珪素原料として、
平均粒径２０〜１７０μｍ、同粒径の標準偏差３５〜６
０μｍにコントロールされたものを使うことによって、
従来に無い高い成形密度の成形体が得られる。これを焼
結することによって、相対密度が９０％以上で１９０Ｗ
／ｍ・Ｋ以上（通常２００Ｗ／ｍ・Ｋ以上）の熱伝導率
のアルミニウム−炭化珪素系複合材料を提供することが
できる。また焼結を熱間鍛造で行うことによって、２４
０Ｗ／ｍ・Ｋ以上のさらに優れた熱伝導性の材料の提供
が可能となる。これら本発明の材料は、パワーモジュー
ル他の半導体装置の放熱基板材料として有利に用いるこ
とができる。As described above, according to the present invention,
In a method for producing an aluminum-silicon carbide composite material in which a metal having aluminum as a main component is a first component and silicon carbide particles are a second component, the content of silicon carbide particles is 6%.
Within the composition range of 0 to 75% by volume, as a silicon carbide raw material,
Average particle size 20 to 170 μm, standard deviation 35 to 6 of the same particle size
By using the one controlled to 0 μm,
A molded body with a high molding density, which has never been seen before, can be obtained. By sintering it, the relative density is 190 W at 90% or more.
/ M · K or more (normally 200 W / m · K or more) can be provided. Further, by performing sintering by hot forging, 24
It is possible to provide a more excellent thermal conductive material of 0 W / m · K or more. These materials of the present invention can be advantageously used as a heat dissipation substrate material for power modules and other semiconductor devices.
【図１】本発明の複合材料を用いた半導体装置の一例を
模式的に示す図である。FIG. 1 is a diagram schematically illustrating an example of a semiconductor device using a composite material of the present invention.
１、本発明の複合材料からなる放熱基板 ２、窒化アルミニウムセラミックスからなる絶縁基板 ３、半導体素子 ４、冷却構造体 1, heat dissipation substrate made of composite material of the present invention 2, insulating substrate made of aluminum nitride ceramics 3, semiconductor element 4, cooling structure
Claims (8)
成分とし、炭化珪素粒子を第二成分とするアルミニウム
−炭化珪素系複合材料であって、該炭化珪素粒子の含有
量が６０〜７５体積％であり、該粒子の平均粒径が２０
〜１７０μｍ、該粒径の標準偏差が３５〜６０μｍであ
るアルミニウム−炭化珪素系複合材料。An aluminum-silicon carbide composite material comprising a metal having aluminum as a main component as a first component and silicon carbide particles as a second component, wherein the content of the silicon carbide particles is 60 to 75 vol. %, And the average particle size of the particles is 20%.
An aluminum-silicon carbide based composite material having a particle size of 35 to 60 μm.
時、相対密度ｙが、（−０．２７ｘ＋１１０）を越える
請求項１に記載のアルミニウム−炭化珪素系複合材料。2. The aluminum-silicon carbide composite material according to claim 1, wherein the relative density y exceeds (−0.27x + 110) when the content of silicon carbide particles is x volume%.
成分とし、炭化珪素粒子を第二成分とするアルミニウム
−炭化珪素系複合材料の製造方法であって、平均粒径が
２０〜１７０μｍ、該粒径の標準偏差が３５〜６０μｍ
である炭化珪素粒子からなる第二成分の粉末６０〜７５
体積％と、第一成分の粉末３５〜４０体積％とを混合し
混合物とする工程と、該混合物を成形し成形体とする工
程と、該成形体を第一成分の融点以上の温度で焼結し焼
結体とする工程とを含むアルミニウム−炭化珪素系複合
材料の製造方法。3. A method for producing an aluminum-silicon carbide composite material comprising a metal having aluminum as a main component as a first component and silicon carbide particles as a second component, wherein the average particle diameter is 20 to 170 μm. Standard deviation of particle size is 35-60 μm
60 to 75 of the second component comprising silicon carbide particles
% Of the first component powder and 35 to 40% by volume of the powder of the first component to form a mixture, molding the mixture to form a compact, and firing the compact at a temperature equal to or higher than the melting point of the first component. Sintering to form a sintered body.
力が４ｔｏｎ／ｃｍ 2以上であり、炭化珪素粒子の含有
量をｘ体積％とした時、該成形体の相対密度ｙを（−
０．２７ｘ＋１１０）％以上とする請求項３に記載のア
ルミニウム−炭化珪素系複合材料の製造方法。4. The method according to claim 1, wherein in the step of forming the molded body, a molding pressure is applied.
Force is 4ton / cm TwoAnd the content of silicon carbide particles
When the amount is x volume%, the relative density y of the molded body is (−
4. The method according to claim 3, wherein the content is 0.27x + 110)% or more.
A method for producing a luminium-silicon carbide composite material.
である請求項４に記載のアルミニウム−炭化珪素系複合
材料の製造方法。5. The method for producing an aluminum-silicon carbide composite material according to claim 4, wherein the molding pressure is 6 ton / cm 2 or more.
って行われる請求項３ないし５のいずれかに記載のアル
ミニウム−炭化珪素系複合材料の製造方法。6. The method for producing an aluminum-silicon carbide composite material according to claim 3, wherein the step of forming the sintered body is performed by hot forging.
2以上である請求項６に記載のアルミニウム−炭化珪素
系複合材料の製造方法。7. The hot forging pressure is 1 ton / cm.
The method for producing an aluminum-silicon carbide composite material according to claim 6, wherein the number is 2 or more.
合材料を用いた半導体装置。8. A semiconductor device using the silicon carbide-based composite material according to claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP24458499A JP2001073048A (en) | 1999-08-31 | 1999-08-31 | Aluminum-silicon carbide composite material and method for producing the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP24458499A JP2001073048A (en) | 1999-08-31 | 1999-08-31 | Aluminum-silicon carbide composite material and method for producing the same |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JP2001073048A true JP2001073048A (en) | 2001-03-21 |
Family
ID=17120903
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP24458499A Pending JP2001073048A (en) | 1999-08-31 | 1999-08-31 | Aluminum-silicon carbide composite material and method for producing the same |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2001073048A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2013237882A (en) * | 2012-05-14 | 2013-11-28 | Furukawa-Sky Aluminum Corp | Method for manufacturing porous aluminum |
| CN117802361A (en) * | 2023-12-29 | 2024-04-02 | 浙江吉成新材股份有限公司 | Ceramic reinforced aluminum-based composite material and preparation method thereof |
-
1999
- 1999-08-31 JP JP24458499A patent/JP2001073048A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2013237882A (en) * | 2012-05-14 | 2013-11-28 | Furukawa-Sky Aluminum Corp | Method for manufacturing porous aluminum |
| CN117802361A (en) * | 2023-12-29 | 2024-04-02 | 浙江吉成新材股份有限公司 | Ceramic reinforced aluminum-based composite material and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| EP0987231B1 (en) | Silicon carbide based composite material and manufacturing method thereof | |
| JP4360061B2 (en) | Semiconductor device member and semiconductor device using the same | |
| US6123895A (en) | Aluminum base member for semiconductor device containing a nitrogen rich surface and method for producing the same | |
| CN100400467C (en) | Heat sink with high thermal conductivity, method for the production thereof and use thereof | |
| JP2000303126A (en) | Diamond-aluminum composite material and method for producing the same | |
| JP3408298B2 (en) | High thermal conductive silicon nitride metallized substrate, method of manufacturing the same, and silicon nitride module | |
| JP2001335859A (en) | Aluminum-silicon carbide based composite material and method for producing the same | |
| JP4314675B2 (en) | Silicon carbide powder, composite material using the same, and manufacturing method thereof | |
| JP4305986B2 (en) | Method for producing silicon carbide composite material | |
| JP2000297301A (en) | Silicon carbide-based composite material, powder thereof, and production method thereof | |
| JP2001180919A (en) | Silicon carbide-carbon composite powder and composite material using the same | |
| JP4253932B2 (en) | Method for producing silicon carbide composite material | |
| JP2001073048A (en) | Aluminum-silicon carbide composite material and method for producing the same | |
| JP4228444B2 (en) | Silicon carbide based composite material and method for producing the same | |
| JP4461513B2 (en) | Aluminum-silicon carbide based composite material and method for producing the same | |
| JP2004169064A (en) | Copper-tungsten alloy, and method of producing the same | |
| JP4275892B2 (en) | Manufacturing method of semiconductor element mounting substrate material | |
| JPH11116361A (en) | Silicon carbide-based composite and heat radiating part using the same | |
| JP4269853B2 (en) | Composite material for substrate for mounting semiconductor element and method for manufacturing the same | |
| US7364692B1 (en) | Metal matrix composite material with high thermal conductivity and low coefficient of thermal expansion | |
| US6972109B1 (en) | Method for improving tensile properties of AlSiC composites | |
| JP2001217364A (en) | Al-SiC COMPOSITE | |
| JP2001284509A (en) | Al-SiC COMPOSITE BODY | |
| JP2001073046A (en) | Method for producing metal-ceramic composite material | |
| JP2001158933A (en) | Al-SiC-based composite material, method of manufacturing the same, and semiconductor device using the same |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A621 | Written request for application examination |
Free format text: JAPANESE INTERMEDIATE CODE: A621 Effective date: 20060322 |
|
| A977 | Report on retrieval |
Free format text: JAPANESE INTERMEDIATE CODE: A971007 Effective date: 20080522 |
|
| A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20080603 |
|
| A02 | Decision of refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A02 Effective date: 20081021 |