JP4850357B2 - Method for producing high thermal conductivity material - Google Patents
Method for producing high thermal conductivity material Download PDFInfo
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- JP4850357B2 JP4850357B2 JP2001194585A JP2001194585A JP4850357B2 JP 4850357 B2 JP4850357 B2 JP 4850357B2 JP 2001194585 A JP2001194585 A JP 2001194585A JP 2001194585 A JP2001194585 A JP 2001194585A JP 4850357 B2 JP4850357 B2 JP 4850357B2
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- thermal conductivity
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- tungsten carbide
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Description
【０００１】
【発明の属する技術分野】
本発明は、高熱伝導性材料の製造方法に関し、特にＩＣパッケージや多層配線基板などに供するヒートシンク材等の放熱体に用いられる高熱伝導性材料の製造方法に関する。
【０００２】
【従来の技術】
半導体、とりわけＬＳＩは、高集積化、高速化されているため発熱が増加しており、それがために、半導体内の回路に誤動作を発生させたり、ひいては半導体回路自身を破壊させたりしている。そのため、高集積半導体を収納するパッケージの熱放散が必要とされている。
【０００３】
そのパッケージの熱放散については、従来、絶縁基板として熱伝導率が約２０Ｗ／ｍＫ程度の熱伝導率の低いアルミナセラミックスからなる材料が用いられているので、熱放散を高めるためにヒートシンクが備えられたパッケージが使用されている。
【０００４】
そのヒートシンクには、高熱伝導性に加えてアルミナセラミックスとの熱膨張係数を一致させるという観点から、その含有割合を変えることにより熱膨張係数を一致させることのでき得る銅とＳｉＣとの複合材料からなるヒートシンクが提案されている。
【０００５】
【発明が解決しようとする課題】
しかしながら、この材料では、複合化はできるものの、ＳｉＣが銅に対して濡れ性が悪いためにＳｉＣと銅との密着性が悪く、それがためにＳｉＣによる銅の拘束が十分に働かないで銅の膨張を抑えることができず、複合化した複合材料の熱膨張係数が思ったより小さくならないという問題があった。
【０００６】
本発明は、上述した材料が有する課題に鑑みなされたものであって、その目的は、高い熱伝導性を維持しつつ、熱膨張係数を低くすることのできる高熱伝導性材料の製造方法を提供することにある。
【０００７】
【課題を解決するための手段】
本発明者等は、上記目的を達成するため鋭意研究した結果、ＳｉＣと銅との複合材料の代わりに炭化タングステン（ＷＣ）と銅との複合材料とすれば、高い熱伝導性を維持しつつ、熱膨張係数の低い高熱伝導性材料が得られるとの知見を得て本発明を完成するに至った。
【０００８】
即ち本発明は、（１）強化材である炭化タングステンを２０〜７０体積％含み、残部が銅からなり、かつ１６０Ｗ／ｍＫ以上の熱伝導率を有し、１０×１０-6／℃以下の熱膨張係数を有することを特徴とする高熱伝導性材料とし、（２） 炭化タングステン粉末で２０〜７０体積％の粉末充填率を有するプリフォームを形成し、そのプリフォームに溶融した銅を不活性ガス雰囲気中で非加圧で浸透させることにより、１６０Ｗ／ｍＫ以上の熱伝導率を有し、１０×１０-6／℃以下の熱膨張係数を有する炭化タングステンと銅との複合材料からなる高熱伝導性材料を作製することを特徴とする高熱伝導性材料の製造方法（請求項１）とすることを要旨とする。以下さらに詳細に説明する。
【０００９】
上記で述べたように、本発明の高熱伝導性材料としては、強化材である炭化タングステンを２０〜７０体積％含み、残部が銅からなり、かつ１６０Ｗ／ｍＫ以上の熱伝導率を有し、１０×１０-6／℃以下の熱膨張係数を有することとする高熱伝導性材料とした。
【００１０】
これは、ＳｉＣの代わりに銅との濡れ性の良い炭化タングステンとすることにより、炭化タングステンと銅との密着性が良くなり、それがために炭化タングステンによる銅の拘束が十分に働いて銅の膨張を抑えることができ、複合化した複合材料の熱膨張係数を期待通り小さくすることができるものとしたものである。
【００１１】
その複合材料中の炭化タングステンの含有率としては、２０〜７０体積％とした。炭化タングステンの含有率が２０体積％より低いと、熱膨張係数が大きくなって低い熱膨張係数が得られず、７０体積％より高いと、高い熱伝導率が得られない。その銅と炭化タングステンとの割合で複合化された材料の熱伝導率は、１６０Ｗ/ｍＫ以上の高い熱伝導率が得られ、１０×１０-6／℃以下の低い熱膨張係数が得られる。
【００１２】
その高熱伝導性材料の製造方法としては、先ず炭化タングステン粉末で２０〜７０体積％の粉末充填率を有するプリフォームを形成し、そのプリフォームに溶融した銅を不活性ガス雰囲気中で非加圧で浸透させることとする製造方法とした（請求項１）。
【００１３】
炭化タングステンと銅とを複合化させる方法としては、慣用の方法が用いられ、例えば、炭化タングステン粉末と銅粉末とを混合し、成形し、焼成して作製する粉末冶金法、炭化タングステン粉末でプリフォームを形成し、そのプリフォームに溶融した銅を加圧して浸透させ作製する高圧鋳造法、あるいはそのプリフォームに溶融した銅を非加圧で浸透させ作製する非加圧浸透法などがある。
【００１４】
その中で非加圧浸透法は、機械的な加圧を行わなくても溶融した銅を浸透できるという特徴があるので、高価で大掛かりな装置を必要とせず、容易で安価に作製できるという特徴があり、しかも炭化タングステンは銅に対する濡れ角が３０°以下とＳｉＣに比べて濡れ性がはるかに良いので、ＳｉＣの場合には難しかったこの非加圧浸透法で簡単に安価に作製できるので、本発明が特に好ましいものとなる。
【００１５】
【発明の実施の形態】
本発明の製造方法を詳しく述べると、ここでは先の非加圧浸透法で製造する方法を述べるので、先ず炭化タングステン粉末を用意し、それに複合化させる銅のインゴットも用意する。
【００１６】
用意した炭化タングステン粉末で２０〜７０体積％の粉末充填率を有するプリフォームを形成する。プリフォームの形成方法はプレス法でもよいし、鋳込み法でもよく、プリフォームを形成できる方法であればどんな方法でもよい。
【００１７】
得られたプリフォームに用意した銅のインゴットを接触させ、それを不活性ガス雰囲気中、例えばアルゴンガス雰囲気中で所定温度で熱処理し、溶融した銅を非加圧でプリフォーム中に浸透させ、それを冷却して炭化タングステンと銅との複合材料からなる高熱伝導性材料を作製する。
【００１８】
以上の方法で高熱伝導性材料を作製すれば、高い熱伝導性を維持しつつ、熱膨張係数の低い高熱伝導性材料が得られる。
【００１９】
【実施例】
以下本発明の実施例を比較例と共に具体的に挙げ、本発明をより詳細に説明する。
【００２０】
（実施例１）
（１）高熱伝導性材料の作製
強化材である炭化タングステン粉末（日本新金属社製、平均粒径１００μｍ）１００重量部にコロイダルシリカ液（常磐電気社製、ＦＪ２９４）を３重量部加え、これにさらにイオン交換水を３０重量部加え混合してスラリーを調整した。
【００２１】
得られたスラリーをフィルタープレスして成形体を成形した後、その成形体を１０００℃の温度で焼成して５０体積％の粉末充填率を有するプリフォームを形成した。得られたプリフォームに銅（平野商店扱い、純度９９．９％）のインゴットを接触させ、それをアルゴンガス雰囲気中で１２００℃の温度で加熱処理し、溶融した銅をプリフォーム中に非加圧で浸透させ、冷却して炭化タングステンと銅との複合材料からなる高熱伝導性材料を作製した。
【００２２】
（２）評価
得られた高熱伝導性材料から３×４×１５ｍｍの試験片を切り出し、その試験片の熱膨張係数をＪＩＳ Ｒ１６１８に準拠して求めた（測定機器：理学電気社製、ＴＭＡ８４１０）。また、得られた高熱伝導性材料からφ１０×２ｍｍの試験片を切り出し、その試験片の熱伝導率をレーザーフラッシュ法で測定した（測定機器：理学電気社製、ＬＦ／ＴＣＭ−ＦＡ８５１０Ｂ）。それらの結果を表１に示す。
【００２３】
（実施例２）
実施例１のフィルタープレス圧を増加して炭化タングステン粉末の充填率を６０体積％とするプリフォームを形成した他は実施例１と同様に高熱伝導性材料を作製し、評価した。その結果も表１に示す。
【００２４】
（比較例１）
比較のために比較例１では、炭化タングステン粉末に銅粉末（昭和化学社製、平均粒径５μｍ）を加えて混合した粉末で炭化タングステン粉末の充填率が１５体積％のプリフォームを形成した他は実施例１と同様に高熱伝導性材料を作製し、評価した。その結果も表１に示す。
【００２５】
（比較例２）
比較のために比較例２では、炭化タングステン粉末に銅粉末（昭和化学社製、平均粒径５μｍ）を加えて混合した粉末をφ２０ｍｍの金型に充填し、それをプレスして成形した成形体をアルゴンガス雰囲気中で１１５０℃の温度で燒結して炭化タングステンの含有率が８５体積％の高熱伝導性材料を作製し、それを実施例１と同様に評価した。その結果も表１に示す。
【００２６】
（比較例３）
比較のために比較例３では、炭化タングステン粉末の代わりにＳｉＣ粉末（信濃電気精錬社製、平均粒径１５μｍ）を用いた他は実施例２と同様に高熱伝導性材料を作製し、評価した。その結果も表１に示す。
【００２７】
【表１】
表１から明らかなように、実施例１、２とも本発明で規定した１６０Ｗ／ｍＫ以上の熱伝導率を有する高熱伝導性材料が得られ、また１０×１０-6 ／℃以下の熱膨張係数を有する高熱伝導性材料が得られた。このことは、本発明の製造方法で製造した高熱伝導性材料であれば、高い熱伝導性を維持しつつ、熱膨張係数を低くすることのできる高熱伝導性材料とすることができることを示している。
【００２９】
これに対して比較例１では、炭化タングステンの含有率が少な過ぎたので、高い熱伝導率が得られるものの、熱膨張係数が本発明の規定した値より大きくなってしまっていた。また、比較例２では、炭化タングステンの含有率が多過ぎたので、低い熱膨張係数が得られるものの、熱伝導率が本発明の規定した値より小さくなってしまっていた。さらに、比較例３では、ＳｉＣによる拘束の働きが十分でないため、熱伝導率は本発明の規定した値より大きくなるものの、熱膨張係数が本発明の規定した値より大きくなってしまっていた。
【００３０】
【発明の効果】
以上の通り、本発明の製造方法で製造した高熱伝導性材料であれば、高い熱伝導性を維持しつつ、熱膨張係数を低くすることのできる高熱伝導性材料とすることができるようになった。このことにより、熱放散のより良好なヒートシンク材等の放熱体に用いられる高熱伝導性材料を提供できるようになった。さらに、非加圧浸透法で作製できるので、複雑な形状のヒートシンク材等であっても、簡単にしかも安価に作製できるようになった。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a process for the preparation of high thermal conductivity materials, more particularly, to a method of manufacturing an IC package and the multilayer wiring substrate such as providing high thermal conductive materials for use in the heat radiator of the heat sink material and the like.
[0002]
[Prior art]
Semiconductors, especially LSIs, have increased heat generation due to higher integration and higher speeds, which causes malfunctions in the circuits in the semiconductors and eventually destroys the semiconductor circuits themselves. . Therefore, there is a need for heat dissipation of a package that houses a highly integrated semiconductor.
[0003]
Regarding the heat dissipation of the package, since a material made of alumina ceramics having a low thermal conductivity of about 20 W / mK is conventionally used as an insulating substrate, a heat sink is provided to increase the heat dissipation. Used packages.
[0004]
From the viewpoint of matching the thermal expansion coefficient with alumina ceramics in addition to high thermal conductivity, the heat sink is made of a composite material of copper and SiC that can match the thermal expansion coefficient by changing the content ratio. A heat sink has been proposed.
[0005]
[Problems to be solved by the invention]
However, although this material can be compounded, SiC has poor wettability to copper, so the adhesion between SiC and copper is poor, which prevents the copper from being restrained sufficiently by SiC. There was a problem that the thermal expansion coefficient of the composite material could not be made smaller than expected.
[0006]
The present invention was made in view of the problems with the above materials is, its object, while maintaining high thermal conductivity, a manufacturing method of the high thermal conductivity materials capable of lowering the thermal expansion coefficient there to be subjected Hisage.
[0007]
[Means for Solving the Problems]
As a result of intensive studies to achieve the above object, the present inventors have maintained a high thermal conductivity if a composite material of tungsten carbide (WC) and copper is used instead of a composite material of SiC and copper. The present invention has been completed with the knowledge that a high thermal conductivity material having a low thermal expansion coefficient can be obtained.
[0008]
That is, the present invention includes (1) 20 to 70% by volume of tungsten carbide as a reinforcing material, the balance is made of copper, and has a thermal conductivity of 160 W / mK or more and 10 × 10 −6 / ° C. or less. and high thermal conductive materials characterized by having a thermal expansion coefficient, (2) to form a preform having a powder filling rate of 20 to 70% by volume of tungsten carbide powder was melted in the preform copper From a composite material of tungsten carbide and copper having a thermal conductivity of 160 W / mK or more and a thermal expansion coefficient of 10 × 10 −6 / ° C. or less by infiltration in an inert gas atmosphere without pressure. The gist of the present invention is to provide a method for producing a high thermal conductivity material (Claim 1 ). This will be described in more detail below.
[0009]
As described above, the high thermal conductivity material of the present invention includes 20 to 70% by volume of tungsten carbide as a reinforcing material, the balance is made of copper, and has a thermal conductivity of 160 W / mK or more. A highly thermally conductive material having a thermal expansion coefficient of 10 × 10 −6 / ° C. or less was obtained.
[0010]
This is because tungsten carbide with good wettability with copper instead of SiC improves the adhesion between tungsten carbide and copper, so that the restraint of copper by tungsten carbide works sufficiently and the copper The expansion can be suppressed, and the thermal expansion coefficient of the composite material can be reduced as expected.
[0011]
The content of tungsten carbide in the composite material was 20 to 70% by volume. When the content of tungsten carbide is lower than 20% by volume, the thermal expansion coefficient becomes large and a low thermal expansion coefficient cannot be obtained. When the content is higher than 70% by volume, high thermal conductivity cannot be obtained. As for the thermal conductivity of the material compounded in the ratio of copper and tungsten carbide, a high thermal conductivity of 160 W / mK or more is obtained, and a low thermal expansion coefficient of 10 × 10 −6 / ° C. or less is obtained.
[0012]
As a method for producing the high thermal conductivity material, first, a preform having a powder filling rate of 20 to 70% by volume is formed with tungsten carbide powder, and the molten copper is non-pressurized in an inert gas atmosphere. ( 1 ).
[0013]
As a method for compounding tungsten carbide and copper, a conventional method is used. For example, a powder metallurgy method in which tungsten carbide powder and copper powder are mixed, molded, and fired, and a tungsten carbide powder is used. There are a high-pressure casting method in which a preform is formed and melted copper is pressed and permeated into the preform, or a non-pressurized infiltration method in which melted copper is permeated into the preform without pressure.
[0014]
Among them, the non-pressure permeation method has the feature that it can permeate the molten copper without performing mechanical pressurization, so it does not require an expensive and large-scale device, and can be easily and inexpensively produced. In addition, tungsten carbide has a wetting angle with respect to copper of 30 ° or less and is much better in wettability than SiC, so it can be easily and inexpensively produced by this non-pressure infiltration method, which was difficult in the case of SiC. The present invention is particularly preferred.
[0015]
DETAILED DESCRIPTION OF THE INVENTION
The manufacturing method of the present invention will be described in detail. Here, since the method of manufacturing by the above-mentioned non-pressurized infiltration method will be described, first, a tungsten carbide powder is prepared, and a copper ingot to be compounded therewith is also prepared.
[0016]
A preform having a powder filling rate of 20 to 70% by volume is formed from the prepared tungsten carbide powder. The forming method of the preform may be a pressing method, a casting method, or any method that can form the preform.
[0017]
A prepared copper ingot is brought into contact with the obtained preform, and it is heat-treated at a predetermined temperature in an inert gas atmosphere, for example, an argon gas atmosphere, and the molten copper is infiltrated into the preform without pressure. It is cooled to produce a highly thermally conductive material made of a composite material of tungsten carbide and copper.
[0018]
If a high thermal conductivity material is produced by the above method, a high thermal conductivity material having a low thermal expansion coefficient can be obtained while maintaining high thermal conductivity.
[0019]
【Example】
Examples of the present invention will be specifically described below together with comparative examples to explain the present invention in more detail.
[0020]
Example 1
(1) Production of a high thermal conductivity material 3 parts by weight of colloidal silica liquid (FJ294, manufactured by Joban Electric Co., Ltd.) is added to 100 parts by weight of tungsten carbide powder (manufactured by Nippon Shin Metals Co., Ltd., average particle size 100 μm). Further, 30 parts by weight of ion exchange water was added and mixed to prepare a slurry.
[0021]
The obtained slurry was filter-pressed to form a formed body, and then the formed body was fired at a temperature of 1000 ° C. to form a preform having a powder filling rate of 50% by volume. The obtained preform is brought into contact with an ingot of copper (treated by Hirano Shoten, purity 99.9%), which is heat-treated at a temperature of 1200 ° C. in an argon gas atmosphere, and the molten copper is not added to the preform. A high thermal conductivity material made of a composite material of tungsten carbide and copper was produced by infiltration with pressure and cooling.
[0022]
(2) Evaluation A 3 × 4 × 15 mm test piece was cut out from the obtained high thermal conductivity material, and the thermal expansion coefficient of the test piece was determined in accordance with JIS R1618 (measuring instrument: RMA, TMA8410). . Moreover, a φ10 × 2 mm test piece was cut out from the obtained high thermal conductivity material, and the thermal conductivity of the test piece was measured by a laser flash method (measuring instrument: LF / TCM-FA8510B, manufactured by Rigaku Corporation). The results are shown in Table 1.
[0023]
(Example 2)
A high thermal conductivity material was prepared and evaluated in the same manner as in Example 1 except that the preform was formed by increasing the filter press pressure of Example 1 to make the filling rate of the tungsten carbide powder 60% by volume. The results are also shown in Table 1.
[0024]
(Comparative Example 1)
For comparison, in Comparative Example 1, a preform in which the filling rate of tungsten carbide powder was 15% by volume was formed by adding and mixing copper powder (made by Showa Chemical Co., Ltd., average particle size 5 μm) with tungsten carbide powder. Were produced and evaluated in the same manner as in Example 1. The results are also shown in Table 1.
[0025]
(Comparative Example 2)
For comparison, in Comparative Example 2, a powder obtained by adding and mixing a tungsten powder with a copper powder (manufactured by Showa Chemical Co., Ltd., average particle size: 5 μm) is filled in a φ20 mm mold, and is molded by pressing it. Was sintered in an argon gas atmosphere at a temperature of 1150 ° C. to produce a highly thermally conductive material having a tungsten carbide content of 85% by volume, which was evaluated in the same manner as in Example 1. The results are also shown in Table 1.
[0026]
(Comparative Example 3)
For comparison, in Comparative Example 3, a highly thermally conductive material was prepared and evaluated in the same manner as in Example 2 except that SiC powder (manufactured by Shinano Denki Seiki Co., Ltd., average particle size 15 μm) was used instead of tungsten carbide powder. . The results are also shown in Table 1.
[0027]
[Table 1]
As is clear from Table 1, a high thermal conductivity material having a thermal conductivity of 160 W / mK or more as defined in the present invention was obtained in both Examples 1 and 2, and a thermal expansion coefficient of 10 × 10 −6 / ° C. or less. A highly thermally conductive material having was obtained. This indicates that a highly thermally conductive material produced by the production method of the present invention can be a highly thermally conductive material capable of reducing the thermal expansion coefficient while maintaining high thermal conductivity. Yes.
[0029]
On the other hand, in Comparative Example 1, since the content of tungsten carbide was too small, a high thermal conductivity was obtained, but the thermal expansion coefficient was larger than the value defined in the present invention. In Comparative Example 2, since the content of tungsten carbide was too large, a low thermal expansion coefficient was obtained, but the thermal conductivity was smaller than the value defined in the present invention. Further, in Comparative Example 3, since the action of restraint by SiC is not sufficient, the thermal conductivity is larger than the value defined in the present invention, but the thermal expansion coefficient is larger than the value defined in the present invention.
[0030]
【The invention's effect】
As described above, if the high thermal conductivity material manufactured by the manufacturing method of the present invention is used, a high thermal conductivity material capable of reducing the thermal expansion coefficient while maintaining high thermal conductivity can be obtained. It was. As a result, it has become possible to provide a highly thermally conductive material used for a heat radiator such as a heat sink material with better heat dissipation. Furthermore, since it can be produced by a non-pressure infiltration method, even a heat sink material having a complicated shape can be produced easily and inexpensively.
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| JP2001194585A JP4850357B2 (en) | 2001-06-27 | 2001-06-27 | Method for producing high thermal conductivity material |
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| JP2001194585A JP4850357B2 (en) | 2001-06-27 | 2001-06-27 | Method for producing high thermal conductivity material |
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| JP2003013168A JP2003013168A (en) | 2003-01-15 |
| JP4850357B2 true JP4850357B2 (en) | 2012-01-11 |
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| CN100443624C (en) * | 2007-02-14 | 2008-12-17 | 西安建筑科技大学 | Preparing technique of activated charcoal carbonide silk net copper-based composite material |
| CN117602909B (en) * | 2024-01-22 | 2024-05-17 | 湖南瑞砂环境科技有限公司 | Floor heating special cement mortar based on tungsten tailings and preparation method thereof |
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