JPH10140262A - Production of metal-ceramics composite material - Google Patents
Production of metal-ceramics composite materialInfo
- Publication number
- JPH10140262A JPH10140262A JP8309960A JP30996096A JPH10140262A JP H10140262 A JPH10140262 A JP H10140262A JP 8309960 A JP8309960 A JP 8309960A JP 30996096 A JP30996096 A JP 30996096A JP H10140262 A JPH10140262 A JP H10140262A
- Authority
- JP
- Japan
- Prior art keywords
- preform
- powder
- metal
- composite material
- aln
- 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
- 239000002131 composite material Substances 0.000 title claims abstract description 57
- 239000000919 ceramic Substances 0.000 title claims abstract description 50
- 238000004519 manufacturing process Methods 0.000 title claims description 17
- 239000000843 powder Substances 0.000 claims abstract description 106
- 238000011049 filling Methods 0.000 claims abstract description 46
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 31
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 23
- 239000000956 alloy Substances 0.000 claims abstract description 23
- 229910052751 metal Inorganic materials 0.000 claims abstract description 17
- 239000002184 metal Substances 0.000 claims abstract description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 11
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 11
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 10
- 239000008119 colloidal silica Substances 0.000 claims abstract description 8
- 239000000835 fiber Substances 0.000 claims abstract description 7
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 6
- 239000002245 particle Substances 0.000 claims description 28
- 238000000034 method Methods 0.000 claims description 27
- 239000012779 reinforcing material Substances 0.000 claims description 17
- 239000007788 liquid Substances 0.000 claims description 14
- 239000000084 colloidal system Substances 0.000 claims description 12
- 238000002360 preparation method Methods 0.000 abstract description 8
- 238000000465 moulding Methods 0.000 abstract description 6
- 230000002787 reinforcement Effects 0.000 abstract description 2
- 239000011369 resultant mixture Substances 0.000 abstract 1
- 238000004078 waterproofing Methods 0.000 abstract 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 47
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 18
- 238000005452 bending Methods 0.000 description 13
- 239000000377 silicon dioxide Substances 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 10
- 238000005470 impregnation Methods 0.000 description 10
- 239000011230 binding agent Substances 0.000 description 8
- 238000011156 evaluation Methods 0.000 description 8
- 229910052757 nitrogen Inorganic materials 0.000 description 8
- 238000001816 cooling Methods 0.000 description 7
- 229910002804 graphite Inorganic materials 0.000 description 6
- 239000010439 graphite Substances 0.000 description 6
- 239000011347 resin Substances 0.000 description 5
- 229920005989 resin Polymers 0.000 description 5
- 229910000838 Al alloy Inorganic materials 0.000 description 4
- 238000005266 casting Methods 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 229920002379 silicone rubber Polymers 0.000 description 4
- 239000004945 silicone rubber Substances 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 229920001187 thermosetting polymer Polymers 0.000 description 4
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 3
- 229910018134 Al-Mg Inorganic materials 0.000 description 3
- 229910018467 Al—Mg Inorganic materials 0.000 description 3
- 229910018566 Al—Si—Mg Inorganic materials 0.000 description 3
- 230000002378 acidificating effect Effects 0.000 description 3
- 239000002585 base Substances 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 229920001971 elastomer Polymers 0.000 description 3
- 238000010304 firing Methods 0.000 description 3
- 238000004663 powder metallurgy Methods 0.000 description 3
- 238000003825 pressing Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000001771 impaired effect Effects 0.000 description 2
- 239000011812 mixed powder Substances 0.000 description 2
- 229920003257 polycarbosilane Polymers 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical group [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 description 1
- 229910000861 Mg alloy Inorganic materials 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000002518 antifoaming agent Substances 0.000 description 1
- LFYJSSARVMHQJB-QIXNEVBVSA-N bakuchiol Chemical compound CC(C)=CCC[C@@](C)(C=C)\C=C\C1=CC=C(O)C=C1 LFYJSSARVMHQJB-QIXNEVBVSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 238000007657 chevron notch test Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000007580 dry-mixing Methods 0.000 description 1
- -1 ductility Chemical class 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 150000002500 ions Chemical group 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000011268 mixed slurry Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000012255 powdered metal Substances 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Landscapes
- Powder Metallurgy (AREA)
- Manufacture Of Alloys Or Alloy Compounds (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、金属に強化材を複
合させた複合材料の製造方法に関し、特に強化材に窒化
アルミニウムの粉末を用いる金属−セラミックス複合材
料の製造方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a composite material in which a metal is combined with a reinforcing material, and more particularly to a method for producing a metal-ceramic composite material using aluminum nitride powder as the reinforcing material.
【０００２】[0002]
【従来の技術】セラミックス繊維または粒子で強化され
た金属−セラミックスの複合材料は、金属とセラミック
スの両方の特性を兼ね備えており、例えばこの複合材料
は、剛性、低熱膨張性、耐摩耗性等のセラミックスの優
れた特性と、延性、高靱性、高熱伝導性等の金属の優れ
た特性を備えている。このように、従来から難しいとさ
れていたセラミックスと金属の両方の特性を備えている
ため、機械装置メーカ等の業界から次世代の材料として
注目されている。2. Description of the Related Art A metal-ceramic composite material reinforced with ceramic fibers or particles has both characteristics of a metal and a ceramic. For example, this composite material has rigidity, low thermal expansion property, abrasion resistance and the like. It has excellent properties of ceramics and excellent properties of metals such as ductility, high toughness, and high thermal conductivity. As described above, since it has both the characteristics of ceramics and metal, which have been considered difficult, it has been drawing attention as a next-generation material from industries such as mechanical device manufacturers.
【０００３】この複合材料、特に金属としてアルミニウ
ムをマトリックスとする複合材料の作製方法は、粉末冶
金法、圧力鋳造法、真空鋳造法等の作製法がある。これ
らの内、粉末冶金法では、粉末状の金属に粒状のあるい
はウィスカー状もしくはファイバー状等のセラミックス
を強化材として混合し、成形し、その成形体を非加圧、
あるいは加圧下で焼成し作製していた。しかしこの方法
で作製された複合材料中の強化材の粉末充填率は、強化
材を多くすると焼結し難くなるため、ウィスカーやファ
イバー状の繊維状のもので最大２５％程度であり、粒子
状のもので最大４０％程度であった。[0003] Methods for producing this composite material, particularly a composite material using aluminum as a matrix as a metal, include powder metallurgy, pressure casting, and vacuum casting. Among them, in powder metallurgy, powdered metal is mixed with granulated or whisker-shaped or fiber-shaped ceramics as a reinforcing material, molded, and the molded body is subjected to non-pressurization.
Alternatively, it was produced by firing under pressure. However, the powder filling rate of the reinforcing material in the composite material produced by this method is at most about 25% for whisker or fibrous fibrous material because sintering becomes difficult when the reinforcing material is increased, and The maximum was about 40%.
【０００４】前記粉末冶金法の他の圧力鋳造法、真空鋳
造法においても、溶解した金属のセラミックス粒子への
濡れ性が悪いため、セラミックス粉末を増やすと金属と
混合し難くなり、強化材の粉末充填率は最大でやはり高
々４０％程度であった。そのため最近では強化材の粉末
充填率を高めるべく、強化材であるセラミックス繊維ま
たは粒子で構成されたプリフォームをあらかじめ形成
し、そのプリフォームに基材である金属を含浸させる含
浸法が採られている。In the pressure casting method and vacuum casting method other than the powder metallurgy method described above, the wettability of the melted metal to the ceramic particles is poor. The filling factor was also at most about 40% at the maximum. Therefore, recently, in order to increase the powder filling rate of the reinforcing material, an impregnation method of forming a preform made of ceramic fibers or particles as the reinforcing material in advance and impregnating the preform with the metal as the base material has been adopted. I have.
【０００５】[0005]
【発明が解決しようとする課題】しかしながら、前記含
浸法においては、プリフォームを構成するセラミックス
が窒化アルミニウム（ＡｌＮ）であると、プリフォーム
の形成に水を用いる場合にはＡｌＮに耐水性がないこと
から使用することはできないという問題があった。一
方、水を用いない場合にはＡｌＮ粉末に熱硬化樹脂を混
合し、それを加熱しながらプレスしてプリフォームを形
成するので、高い粉末充填率を有する複合材料が得られ
ないこと、プレス機等の設備が必要となり、製造コスト
が高くなることなどの問題があった。特に大型品を作製
するには、高価なプレス機が必要となり一層コスト高と
なる。また、有機ケイ素系の熱硬化樹脂を使用している
ので、溶湯アルミニウムが含浸する過程で樹脂中のケイ
素成分がマトリックス中に生成するため、曲げ強度、破
壊靱性などの特性が低下するという問題もあった。However, in the above-mentioned impregnation method, if the ceramic constituting the preform is aluminum nitride (AlN), the water is not used in forming the preform when AlN is used. There was a problem that it could not be used. On the other hand, when water is not used, the thermosetting resin is mixed with the AlN powder and pressed while heating to form a preform. Therefore, a composite material having a high powder filling rate cannot be obtained. There is a problem that equipment such as the above is required and the manufacturing cost is increased. In particular, in order to produce a large product, an expensive press machine is required, which further increases the cost. In addition, since the organosilicon-based thermosetting resin is used, the silicon component in the resin is generated in the matrix during the process of impregnating the molten aluminum, which causes a problem that properties such as bending strength and fracture toughness are reduced. there were.
【０００６】本発明は、上述した含浸法による金属−セ
ラミックス複合材料の製造方法が有する課題に鑑みなさ
れたものであって、その目的は、強化材として窒化アル
ミニウムを用いても問題なく製造することができる金属
−セラミックス複合材料の製造方法を提供することにあ
る。The present invention has been made in view of the problems of the above-described method for producing a metal-ceramic composite material by the impregnation method, and an object of the present invention is to produce a metal-ceramic composite material without any problem even if aluminum nitride is used as a reinforcing material. It is an object of the present invention to provide a method for producing a metal-ceramic composite material that can be used.
【０００７】[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、粉末充填率が３０〜
６０ｖｏｌ％のプリフォームについては、ＡｌＮ粉末を
カーボン等の容器中に充填する方法で、粉末充填率が６
０〜８０ｖｏｌ％のプリフォームについては、耐水処理
を施したＡｌＮ粉末にコロイダルシリカ液または／及び
アルミナ水和物のコロイド液を加え成形した後、その成
形体を焼成する方法でプリフォームを形成することと
し、その形成したプリフォームに金属を含浸すれば、Ａ
ｌＮ粉末を用いても、含浸法で問題なく金属−セラミッ
クス複合材料を製造できるとの知見を得て本発明を完成
した。Means for Solving the Problems The inventors of the present invention have conducted intensive studies to achieve the above object, and as a result, the powder filling rate was 30 to
For a preform of 60 vol%, a method of filling AlN powder into a container such as carbon has a powder filling rate of 6%.
For a preform of 0 to 80 vol%, a colloidal silica solution or / and a colloidal solution of alumina hydrate are added to a water-resistant AlN powder, molded, and then the molded body is fired to form a preform. If the formed preform is impregnated with metal, A
The present inventors have found that a metal-ceramic composite material can be produced by the impregnation method without any problem even if 1N powder is used, thereby completing the present invention.
【０００８】即ち本発明は、（１）セラミックス繊維ま
たは粒子を強化材としてプリフォームを形成し、そのプ
リフォームに基材である金属を含浸させる金属−セラミ
ックス複合材料の製造方法において、該プリフォーム
が、１〜１００μｍの平均粒径を有し、３０〜６０ｖｏ
ｌ％の粉末充填率を有するＡｌＮ粉末から成り、該プリ
フォームの形成方法が、ＡｌＮ粉末をカーボン等の容器
中に充填して形成する方法であるとし、その形成された
プリフォームにアルミニウムを主成分とする合金を７０
０〜１０００℃の温度で含浸させることを特徴とする金
属−セラミックス複合材料の製造方法（請求項１）と
し、また、（２）セラミックス繊維または粒子を強化材
としてプリフォームを形成し、そのプリフォームに基材
である金属を含浸させる金属−セラミックス複合材料の
製造方法において、該プリフォームが、１〜１００μｍ
の平均粒径を有し、６０〜８０ｖｏｌ％の粉末充填率を
有する耐水処理を施したＡｌＮ粉末から成り、該プリフ
ォームの形成方法が、ＡｌＮ粉末にコロイダルシリカ液
または／及びアルミナ水和物のコロイド液を加え成形し
た後、その成形体を焼成する方法であるとし、その形成
されたプリフォームにアルミニウムを主成分とする合金
を７００〜１０００℃の温度で含浸させることを特徴と
する金属−セラミックス複合材料の製造方法（請求項
２）とすることを要旨とする。以下さらに詳細に説明す
る。That is, the present invention relates to (1) a method for producing a metal-ceramic composite material in which a preform is formed using ceramic fibers or particles as a reinforcing material, and the preform is impregnated with a metal as a base material. Has an average particle size of 1 to 100 μm, and 30 to 60 vo
It is assumed that the preform is formed by filling AlN powder into a container such as carbon or the like, and aluminum is mainly used in the formed preform. 70 as the component alloy
A method for producing a metal-ceramic composite material characterized by being impregnated at a temperature of 0 to 1000 ° C. (Claim 1). (2) A preform is formed by using ceramic fibers or particles as a reinforcing material. In a method for producing a metal-ceramic composite material in which a metal as a base material is impregnated in a reform, the preform is 1 to 100 μm
And a water-resistant AlN powder having a powder filling rate of 60 to 80 vol%, and the method of forming the preform is performed by adding a colloidal silica liquid or / and alumina hydrate to the AlN powder. The method is characterized in that the method comprises a step of baking the formed body after adding and forming a colloid liquid, and impregnating the formed preform with an alloy containing aluminum as a main component at a temperature of 700 to 1000 ° C. The gist of the present invention is a method of manufacturing a ceramic composite material (claim 2). This will be described in more detail below.
【０００９】上記（１）のプリフォームとしては、１〜
１００μｍの平均粒径を有し、３０〜６０ｖｏｌ％の粉
末充填率を有するＡｌＮ粉末から成るプリフォームと
し、そのプリフォームの形成方法としては、ＡｌＮ粉末
をカーボン等の容器中に充填して形成する方法とした。
ＡｌＮ粉末の平均粒径を１〜１００μｍとしたのは、こ
の範囲でないと堅固なプリフォームにし難いことによ
る。さらに、粉末充填率を３０〜６０ｖｏｌ％としたの
は、この範囲のプリフォームであれば容易に形成するこ
とができることによる。As the preform of the above (1),
A preform made of AlN powder having an average particle diameter of 100 μm and a powder filling rate of 30 to 60 vol% is formed. The preform is formed by filling the AlN powder into a container such as carbon. Method.
The reason why the average particle diameter of the AlN powder is 1 to 100 μm is that it is difficult to form a solid preform outside this range. Further, the reason for setting the powder filling rate to 30 to 60 vol% is that a preform in this range can be easily formed.
【００１０】上記ＡｌＮ粉末の純度としては、９８％以
上が好ましいが、ＡｌＮの特徴である耐プラズマ性、高
熱伝導性等が損なわれない範囲の純度であればよい。ま
た、ＡｌＮの特性を損なわなければ他の種類の粉末を１
０ｗｔ％以下であれば混合してもよく、例えば耐プラズ
マ性を重視すればＡｌ2Ｏ3粉末を１０ｗｔ％以下なら混
合してもよく、高熱伝導性を重視すればＳｉＣ、ＢＮ等
の熱伝導性の良好な粉末を１０ｗｔ％以下なら混合して
もよい。[0010] The purity of the AlN powder is preferably 98% or more, but may be any purity as long as the characteristics of AlN such as plasma resistance and high thermal conductivity are not impaired. If the characteristics of AlN are not impaired, another type of powder may be used.
If it is 0 wt% or less, it may be mixed. For example, if plasma resistance is emphasized, Al 2 O 3 powder may be mixed if it is 10 wt% or less. If high thermal conductivity is emphasized, thermal conductivity of SiC, BN, or the like may be used. If a powder having good properties is 10 wt% or less, it may be mixed.
【００１１】上記カーボン等の材料としては、通常のグ
ラファイト部材、またはグラファイトをシート状にした
もの等金属を含浸している途中でＡｌと反応もしくは容
器自体が溶解しない材料であればよく、例えばカーボン
の他ステンレス等の材料も使用することができる。シー
ト状のものは、形状を自由に変えられるので好ましく、
その厚さは、１ｍｍ以下が種々の形状の容器を作製する
のに好ましい。作製した容器に粉末を充填してプリフォ
ームを形成するが、充填する際に充填率が向上するよう
に振動を加えてもよい。このように、容器に粉末を充填
しただけでプリフォームとするので、プリフォームの粉
末充填率を６０ｖｏｌ％以上と高くすることは難しい
が、水を使う必要もなく、また特別の設備を必要としな
いので、プリフォームを安価で容易に形成することがで
きる。The material such as carbon may be any material which does not react with Al or dissolve the container itself during the impregnation of a metal such as a normal graphite member or a sheet of graphite. Other materials such as stainless steel can also be used. Sheet-shaped objects are preferred because the shape can be changed freely,
The thickness of 1 mm or less is preferable for producing containers of various shapes. The preform is formed by filling the prepared container with the powder, and vibration may be applied during filling so as to improve the filling rate. As described above, it is difficult to increase the preform powder filling rate to 60 vol% or more because the preform is formed only by filling the container with the powder, but there is no need to use water and special equipment is required. Therefore, the preform can be easily formed at low cost.
【００１２】また、上記（２）のプリフォームとして
は、１〜１００μｍの平均粒径を有し、６０〜８０ｖｏ
ｌ％の粉末充填率を有する耐水処理を施したＡｌＮ粉末
から成るプリフォームとし、そのプリフォームの形成方
法としては、耐水処理を施したＡｌＮ粉末にコロイダル
シリカ液または／及びアルミナ水和物のコロイド液を加
え成形した後、その成形体を焼成する方法とした。Ａｌ
Ｎ粉末の平均粒径を１〜１００μｍとしたのは、前記し
たと同じであり、さらに、粉末充填率を６０〜８０ｖｏ
ｌ％としたのは、上記（１）では難しい高い範囲の粉末
充填率を有するプリフォームを容易に形成することがで
きることによる。The preform of the above (2) has an average particle diameter of 1 to 100 μm, and has an average particle size of 60 to 80 vo.
A preform made of a water-resistant AlN powder having a powder filling rate of 1% is prepared. The preform is formed by adding a colloid of a colloidal silica liquid or / and alumina hydrate to the water-resistant AlN powder. After molding by adding a liquid, the molded body was fired. Al
The reason why the average particle diameter of the N powder is set to 1 to 100 μm is the same as described above, and further, the powder filling rate is set to 60 to 80 vol.
The reason why the amount is set to 1% is that a preform having a powder filling rate in a high range, which is difficult in the above (1), can be easily formed.
【００１３】上記（２）のプリフォームの形成方法が水
を用いる方法であるので、用いるＡｌＮ粉末としては、
耐水処理を施したＡｌＮ粉末とした。耐水処理として
は、ＣＶＤ、ＰＶＤ処理して粉末表面にコーティングし
てもよく、ナイロン等の水溶性でない有機物を表面にコ
ーティング処理してもよい。耐水処理していないＡｌＮ
粉末を用いると、直ちに水と反応して水酸化アルミニウ
ム、アンモニアを生成しＡｌＮとして残存しない。Ａｌ
Ｎ粉末の純度としては、前記したと同じく、また、Ａｌ
Ｎ粉末に他の種類の粉末を混合するのも前記したと同じ
である。Since the method of forming a preform of the above (2) is a method using water, the AlN powder used is as follows:
The AlN powder was subjected to a water-resistant treatment. As the water-resistant treatment, the powder surface may be coated by CVD or PVD treatment, or a non-water-soluble organic substance such as nylon may be coated on the surface. AlN without water resistance treatment
When the powder is used, it reacts immediately with water to produce aluminum hydroxide and ammonia and does not remain as AlN. Al
As for the purity of the N powder, as described above,
Mixing another type of powder with N powder is the same as described above.
【００１４】上記プリフォームの形成に用いるバインダ
ーとしては、コロイダルシリカ液または／及びアルミナ
水和物のコロイド液とした。これらをバインダーとした
のは、粉末充填率が高く、かつ金属を含浸するに十分な
強度を有するプリフォームとすることができることによ
る。以下に各バインダーをさらに詳細に説明する。The binder used for forming the preform was a colloidal silica solution or a colloidal solution of alumina hydrate. The reason for using these as binders is that a preform having a high powder filling rate and sufficient strength to impregnate metal can be obtained. Hereinafter, each binder will be described in more detail.
【００１５】コロイダルシリカ液は、アルカリ領域で安
定なシリカ液と酸性領域で安定なシリカ液とがあり、ア
ルカリ領域で安定なシリカ液では、Ｎａ等で安定化した
コロイドの大きさが５〜５０ｎｍのシリカ液を用いるこ
とができる。液中のシリカの濃度は１０〜４０ｗｔ％程
度の範囲にあり、安定化剤のアルカリ成分の濃度として
は、Ｎａ2Ｏ換算で０．４ｗｔ％以下が好ましい。これ
以上の濃度であるとＮａイオンによりプリフォームに含
浸してきたＡｌがＡｌ2Ｏ3化し易くなり、プリフォーム
は高強度になるが、複合体の特性、特に曲げ強度、破壊
靱性が低下するので好ましくない。また、ＡｌＮの粒界
がガラス化して閉気孔となり易く含浸の阻害となる。The colloidal silica liquid includes a silica liquid which is stable in an alkaline region and a silica liquid which is stable in an acidic region. In a silica liquid which is stable in an alkaline region, the size of a colloid stabilized with Na or the like is 5 to 50 nm. Can be used. The concentration of silica in the liquid is in the range of about 10 to 40 wt%, and the concentration of the alkali component of the stabilizer is preferably 0.4 wt% or less in terms of Na 2 O. If the concentration is higher than this, Al impregnated into the preform by Na ions is easily converted to Al 2 O 3, and the preform becomes high in strength, but the properties of the composite, particularly, the bending strength and the fracture toughness are reduced. Not preferred. In addition, the grain boundaries of AlN are vitrified to form closed pores, which hinders impregnation.
【００１６】一方、酸性領域で安定なシリカ液では、酸
性で安定したコロイドの大きさが５〜５０ｎｍのシリカ
液を用いることができる。液中のシリカの濃度は前記し
たと同じく１０〜４０ｗｔ％程度の範囲にあり、アルカ
リ成分の濃度は、Ｎａ2Ｏ換算で０．０５以下が好まし
い。On the other hand, in the case of a silica liquid which is stable in an acidic region, an acidic and stable colloid having a colloid size of 5 to 50 nm can be used. The concentration of silica in the liquid is in the range of about 10 to 40 wt% as described above, and the concentration of the alkali component is preferably 0.05 or less in terms of Na 2 O.
【００１７】次に、アルミナ水和物のコロイド液は、コ
ロイドの大きさが１〜１０００ｎｍで、Ｃｌ-、ＣＨ3Ｃ
ＯＯ-もしくはＮＯ3 -で安定化したコロイド液を用いる
ことができる。このアルミナ水和物のコロイド液と前記
したコロイダルシリカ液とを混合して用いることもでき
る。混合の目安としては、シリカ成分の割合がアルミナ
成分に対し、１０〜８０ｗｔ％程度とする。これらバイ
ンダーをＡｌＮ粉末に適量加え成形し、焼成することで
プリフォームを形成することができる。このように、耐
水性を有したＡｌＮ粉末を用い、その粉末を前記バイン
ダーで結合させたプリフォームとするので、水を使って
も問題なく粉末充填率が６０ｖｏｌ％以上のプリフォー
ムを容易に形成することができる。Next, colloidal solution of alumina hydrate, the size of the colloid in 1~1000nm, Cl -, CH 3 C
OO - or NO 3 - stabilized colloidal solution can be used. This colloidal solution of alumina hydrate and the above-mentioned colloidal silica solution can be used in combination. As a guide for mixing, the ratio of the silica component is about 10 to 80 wt% with respect to the alumina component. A preform can be formed by adding an appropriate amount of these binders to AlN powder, molding and firing. As described above, since the AlN powder having water resistance is used to form the preform in which the powder is bonded with the binder, a preform having a powder filling rate of 60 vol% or more can be easily formed without using water. can do.
【００１８】プリフォームに金属を含浸する方法として
は、アルミニウムを主成分とする合金を７００〜１００
０℃の温度で含浸させることとした。金属をアルミニウ
ム合金としのは、ＡｌＮ粉末に濡れ性がよく好ましいこ
とによる。この合金の含浸温度は、この範囲より低いと
合金が溶解せず、この範囲より高いとＡｌが酸化し好ま
しくない。このアルミニウムの種類としては、Ａｌ単味
を含め、Ａｌ−Ｓｉ−Ｍｇ系、Ａｌ−Ｍｇ系のアルミニ
ウム合金等があり、いずれのものでも使用することがで
きる。As a method of impregnating the preform with a metal, an alloy containing aluminum as a main component is 700 to 100%.
The impregnation was performed at a temperature of 0 ° C. The reason why the metal is aluminum alloy is that AlN powder has good wettability and is preferable. If the impregnation temperature of this alloy is lower than this range, the alloy does not melt, and if it is higher than this range, Al is oxidized, which is not preferable. Examples of the type of aluminum include Al-Si-Mg-based and Al-Mg-based aluminum alloys, including Al alone, and any of them can be used.
【００１９】[0019]
【発明の実施の形態】本発明の製造方法をさらに詳しく
述べると、先ず強化材として１〜１００μｍの平均粒径
を有するＡｌＮ粉末、またはそれにＡｌ2Ｏ3等のセラミ
ックス粉末を１０％以下混合した粉末を用いる。ＡｌＮ
粉末は単一の粒径のものでもよいが、２種類の粒径の粉
末を混合した方が充填率が高くなり成形体の強度が増加
するので望ましい。More particularly the manufacturing method of the embodiment of the present invention, the first AlN powder having an average particle size of 1 to 100 [mu] m, or in the ceramic powder of Al 2 O 3 or the like by mixing 10% or less as reinforcement Use powder. AlN
The powder may be of a single particle size, but it is desirable to mix powders of two types of particle size because the filling rate increases and the strength of the molded body increases.
【００２０】次いで、上記（１）の製造方法では、グラ
ファイトシート等を用いて所望の形状の容器を作製す
る。作製した容器にＡｌＮ粉末を振動を加え、あるいは
加えないで充填してプリフォームを形成する。そのプリ
フォームに窒素気流中で非加圧、あるいは加圧して７０
０〜１０００℃の温度でＡｌ、またはＡｌ−Ｓｉ−Ｍｇ
系あるいはＡｌ−Ｍｇ系のアルミニウム合金を含浸させ
る。Next, in the manufacturing method (1), a container having a desired shape is manufactured using a graphite sheet or the like. The prepared container is filled with AlN powder with or without vibration to form a preform. Non-pressurizing or pre-pressing the preform in a nitrogen stream
Al or Al-Si-Mg at a temperature of 0 to 1000 ° C
System or an Al-Mg system aluminum alloy.
【００２１】また、上記（２）の製造方法では、先ず上
述のＡｌＮ粉末に前記した耐水処理を施し、その耐水処
理したＡｌＮ粉末に対し、イオン交換水を１０〜５０ｗ
ｔ％程度、前記したバインダーを０．１〜３０ｗｔ％程
度、そのほか必要があれば消泡剤を２ｗｔ％程度以下、
尿素を２ｗｔ％程度以下加える。バインダーの量は、少
ないと作製したプリフォームの強度が低く複合化する際
に支障を生じ、多すぎると閉気孔を生じて複合化できな
い。In the method (2), the AlN powder is first subjected to the above-mentioned water-resistant treatment, and ion-exchanged water is added to the water-resistant AlN powder for 10 to 50 watts.
about t%, about 0.1 to 30 wt% of the binder, and about 2 wt% or less of an antifoaming agent if necessary.
Urea is added at about 2 wt% or less. If the amount of the binder is too small, the strength of the produced preform is low, which hinders the formation of a composite, and if the amount is too large, closed pores are formed and the composite cannot be formed.
【００２２】得られた配合物をポットミルで１時間以上
混合するが、あまり長いと粒子表面に施した耐水処理層
が劣化してＡｌＮ表面が露出し水と反応することになる
ので、５０時間以内が望ましい。また、ポットミルにボ
ールを入れるのは、前記した問題が顕著となり好ましく
ない。混合したスラリーは、振動を印加して沈降成形、
すなわちセディメントキャストする。スラリーの粘度
は、粘性が高いと粉末が沈降しないため、１００ポイズ
以下が望ましい。通常はシリコーンゴム型を使用する
が、プラスチック、アルミニウム等の型であってもよ
く、特に限定はない。粒子が沈降する間はなるべく振動
を加え充填をよくする。得られた成形体は冷凍して脱型
する。冷凍は水が凍ればよく温度に限定はない。脱型し
た成形体を７０〜１３０℃の温度で乾燥する。この乾燥
した状態でも成形体の強度をある程度発現できるので、
必要に応じプリフォームとして用いてもよいが、通常は
４００〜１１００℃の温度で焼成してプリフォームとす
る。The obtained composition is mixed in a pot mill for 1 hour or more. If it is too long, the water-resistant treatment layer applied to the particle surface is deteriorated, and the AlN surface is exposed and reacts with water. Is desirable. In addition, putting a ball in a pot mill is not preferable because the above-mentioned problem is remarkable. The mixed slurry is settled by applying vibration,
That is, sediment cast is performed. The viscosity of the slurry is preferably 100 poise or less because the powder does not settle if the viscosity is high. Normally, a silicone rubber mold is used, but a mold of plastic, aluminum or the like may be used, and there is no particular limitation. During the sedimentation of the particles, vibration is applied as much as possible to improve the filling. The obtained compact is frozen and demolded. Freezing is not limited as long as the water is frozen. The demolded compact is dried at a temperature of 70 to 130C. Since the strength of the molded body can be expressed to some extent even in this dry state,
Although it may be used as a preform if necessary, it is usually fired at a temperature of 400 to 1100 ° C. to obtain a preform.
【００２３】得られたプリフォームに窒素気流中で非加
圧、あるいは加圧して７００〜１０００℃の温度でＡ
ｌ、Ａｌ−Ｓｉ−Ｍｇ系またはＡｌ−Ｍｇ系のアルミニ
ウム合金を含浸させる。含浸させた後、そのまま炉内で
１０〜３００℃／ｈの降温速度で冷却する。冷却の際、
熱歪の発生を抑えるためにマトリックスが固化する途中
の温度で１〜１０時間程度保持してもよい。The obtained preform is not pressurized in a nitrogen stream or pressurized at a temperature of 700 to 1000 ° C.
1, impregnated with an Al-Si-Mg-based or Al-Mg-based aluminum alloy. After impregnation, it is cooled in a furnace at a temperature lowering rate of 10 to 300 ° C / h. Upon cooling,
In order to suppress the occurrence of thermal strain, the matrix may be maintained at a temperature during solidification of the matrix for about 1 to 10 hours.
【００２４】以上の方法で金属−セラミックス複合材料
を作製すれば、ＡｌＮ粉末を用いても、安価でまた粉末
充填率の高いものを含んだ金属−セラミックス複合材料
が得られる。If a metal-ceramic composite material is produced by the above-described method, a metal-ceramic composite material which is inexpensive and contains a high powder filling rate can be obtained even if AlN powder is used.
【００２５】[0025]
【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。EXAMPLES Hereinafter, the present invention will be described in more detail with reference to Examples of the present invention and Comparative Examples.
【００２６】（実施例１） （１）金属−セラミックス複合材料の作製 ０．８ｍｍの厚さのグラファイトシートを用いて５００
×５００×３０ｍｍの箱を作製し、その中に平均粒径が
１６μｍのＡｌＮ粉末を振動を加えながら高さが１０ｍ
ｍとなるよう充填しプリフォームを作製した。得られた
プリフォームの上面に２００μｍ程度の大きさのＭｇ粉
末を２００ｇふりかけ、その上にＡｌ−５Ｍｇの合金を
４ｋｇ載置し、８１０℃窒素気流中（２０リットル／ｍ
ｉｎ：炉内容積０．４０ｍ3）でプリフォームに合金を
含浸させた後、炉内で１００℃／ｈの降温速度で７００
℃まで冷却し、その温度で１時間保持してから再度１０
０℃／ｈで室温まで冷却して金属−セラミックスの複合
材料を作製した。(Example 1) (1) Production of metal-ceramic composite material 500 parts were prepared using a 0.8 mm thick graphite sheet.
A box of × 500 × 30 mm is prepared, and an AlN powder having an average particle size of 16 μm is placed in the box with a height of 10 m while applying vibration.
m to prepare a preform. 200 g of Mg powder having a size of about 200 μm is sprinkled on the upper surface of the obtained preform, and 4 kg of an Al-5Mg alloy is placed on the Mg powder and placed in a nitrogen stream at 810 ° C. (20 l / m 2).
in: After the preform was impregnated with the alloy at a furnace volume of 0.40 m 3 ), the temperature was lowered at a rate of 100 ° C./h in the furnace at 700 ° C.
° C, hold at that temperature for 1 hour, and
It was cooled to room temperature at 0 ° C./h to produce a metal-ceramic composite material.
【００２７】（２）評価 得られたプリフォームの粉末充填率をプリフォームの重
量と外形寸法より求めた。また、得られた複合材料の曲
げ強度をＪＩＳ Ｒ１６０１により求め、さらに別にシ
ェブロンノッチを導入した試験片を作製し、その試験片
で同じくＪＩＳＲ１６０１により曲げ強度を求め、その
値から破壊靱性値を求めた。それらの結果を表１に示
す。(2) Evaluation The powder filling rate of the obtained preform was determined from the weight and external dimensions of the preform. Further, the bending strength of the obtained composite material was determined by JIS R1601, a test piece into which a chevron notch was introduced was further prepared, and the bending strength of the test piece was also determined by JIS R1601, and the fracture toughness was determined from the value. . Table 1 shows the results.
【００２８】（実施例２） （１）金属−セラミックス複合材料の作製 グラファイトブロックから７００×８００×５０ｍｍの
箱を作製し、その内側に０．３ｍｍの厚さのグラファイ
トシートを貼り付け、その底に２００μｍ程度の大きさ
のＭｇ粉末をふりかけた。その箱の中に平均粒径が１６
μｍと２５μｍのＡｌＮ粉末を１：１で乾式混合した混
合粉末を充填にムラが生じないように板で上から押しな
がら高さが１５ｍｍとなるように充填しプリフォームを
作製した。得られたプリフォームの上面にＡｌ−２Ｍｇ
の合金を１２ｋｇ載置し、８３０℃窒素気流中（２０リ
ットル／ｍｉｎ：炉内容積０．４０ｍ3）でプリフォー
ムに合金を含浸させた後、実施例１と同様に冷却して金
属−セラミックスの複合材料を作製した。Example 2 (1) Preparation of Metal-Ceramic Composite Material A 700 × 800 × 50 mm box was prepared from a graphite block, and a 0.3 mm thick graphite sheet was adhered to the inside of the box. Was sprinkled with Mg powder having a size of about 200 μm. The average particle size in the box is 16
A preform was prepared by filling a mixed powder obtained by dry mixing 1 μm and 25 μm AlN powder at a ratio of 1: 1 while pressing from above with a plate so as to prevent unevenness. Al-2Mg on the upper surface of the obtained preform
Is placed in a nitrogen stream at 830 ° C. (20 l / min: furnace volume 0.40 m 3 ), and then impregnated with the alloy. Was prepared.
【００２９】（２）評価 得られたプリフォームの粉末充填率、複合材料の曲げ強
度、破壊靱性値を実施例１と同様に求めた。それらの結
果も表１に示す。(2) Evaluation The powder filling rate of the obtained preform, the bending strength of the composite material, and the fracture toughness were determined in the same manner as in Example 1. The results are also shown in Table 1.
【００３０】（実施例３） （１）金属−セラミックス複合材料の作製 ステンレスを用いて６００×５００×１００ｍｍの箱を
作製し、その中に平均粒径が２５μｍのＡｌＮ粉末を振
動を加えながら高さが８０ｍｍとなるように充填しプリ
フォームを作製した。得られたプリフォームの上面に２
００μｍ程度の大きさのＭｇ粉末を１００ｇふりかけ、
その上に純度が９８％以上のＡｌを１０ｋｇ載置し、８
８０℃窒素気流中（２０リットル／ｍｉｎ：炉内容積
０．４０ｍ3）でプリフォームに合金を含浸させた後、
実施例１と同様に冷却して金属−セラミックスの複合材
料を作製した。Example 3 (1) Preparation of Metal-Ceramic Composite Material A 600 × 500 × 100 mm box was prepared using stainless steel, and an AlN powder having an average particle diameter of 25 μm was placed in the box while applying vibration to the box. To obtain a preform. 2 on the upper surface of the obtained preform
Sprinkle 100g of Mg powder of about 00μm size,
10 kg of Al having a purity of 98% or more is placed on the
After the alloy was impregnated into the preform at 80 ° C. in a nitrogen stream (20 l / min: furnace volume 0.40 m 3 ),
Cooling was performed in the same manner as in Example 1 to produce a metal-ceramic composite material.
【００３１】（２）評価 得られたプリフォームの粉末充填率、複合材料の曲げ強
度、破壊靱性値を実施例１と同様に求めた。それらの結
果も表１に示す。(2) Evaluation The powder filling ratio of the obtained preform, the bending strength of the composite material, and the fracture toughness were determined in the same manner as in Example 1. The results are also shown in Table 1.
【００３２】（比較例１） （１）金属−セラミックス複合材料の作製 ５０×５０×１０ｍｍの金型に、平均粒径が１６μｍの
ＡｌＮ粉末にポリカルボシラン等の熱硬化性樹脂を５ｗ
ｔ％加えて混合した粉末を充填し、その粉末に２００℃
で２トンの荷重を１時間加えて成形し、その成形体を空
気中で４５０℃で焼成しプリフォームを作製した。得ら
れたプリフォームの上面に２００μｍ程度の大きさのＭ
ｇ粉末を１ｇふりかけ、その上にＡｌ−５Ｍｇの合金を
１５０ｇ載置し、８２０℃窒素気流中（２０リットル／
ｍｉｎ：炉内容積０．４０ｍ3）でプリフォームに合金
を含浸させた後、実施例１と同様に冷却して金属−セラ
ミックスの複合材料を作製した。Comparative Example 1 (1) Preparation of Metal-Ceramic Composite Material In a mold of 50 × 50 × 10 mm, a thermosetting resin such as polycarbosilane was added to AlN powder having an average particle diameter of 16 μm for 5 watts.
t% and the mixed powder is filled, and the powder
Then, a load of 2 tons was applied for 1 hour, and the formed body was fired at 450 ° C. in air to produce a preform. On the upper surface of the obtained preform, a size of about 200 μm M
1 g of powder, sprinkle 1 g of the powder, and place 150 g of the Al-5Mg alloy on top of it, in a nitrogen stream at 820 ° C. (20 liters /
min: a furnace volume of 0.40 m 3 ) was impregnated with the alloy in the preform, and then cooled as in Example 1 to produce a metal-ceramic composite material.
【００３３】（２）評価 得られたプリフォームの粉末充填率、複合材料の曲げ強
度、破壊靱性値を実施例１と同様に求めた。それらの結
果も表１に示す。(2) Evaluation The powder filling ratio of the obtained preform, the bending strength of the composite material, and the fracture toughness were determined in the same manner as in Example 1. The results are also shown in Table 1.
【００３４】（実施例４） （１）金属−セラミックス複合材料の作製 平均粒径が１５μｍの表面にシリカをコーティングした
ＡｌＮ粉末に対し、イオン交換水を２４ｗｔ％、固形分
濃度が２０％のアルミナ水和物のコロイド液（コロイド
の大きさは１０×２０ｎｍ）を１０ｗｔ％加え、ボール
を入れてないポットミルで２時間混合した。得られたス
ラリーを１８０×２５×２５ｍｍの大きさのシリコーン
ゴム型に流し込み、１時間振動を印加して強化材を沈降
させ成形した。成形後、ゴム型ごと−２５℃に冷却し冷
凍して脱型した。脱型後、８０℃で２４時間乾燥した
後、５０℃／ｈの昇温速度で大気雰囲気中で４５０℃で
５時間焼成した後、５０℃／ｈの降温速度で室温まで冷
却してプリフォームを作製した。得られたプリフォーム
の上にプリフォームと同重量のＡｌ−５Ｍｇの合金を載
置し、８２５℃窒素気流中（２０リットル／ｍｉｎ：炉
内容積０．４０ｍ3）でプリフォームに合金を含浸させ
た後、実施例１と同様に冷却して金属−セラミックスの
複合材料を作製した。Example 4 (1) Preparation of Metal-Ceramic Composite Material Alumina having 24% by weight of ion-exchanged water and 20% of solid content was added to AlN powder having an average particle size of 15 μm coated with silica. A hydrate colloid solution (colloid size: 10 × 20 nm) was added at 10 wt%, and mixed for 2 hours in a pot mill without a ball. The obtained slurry was poured into a silicone rubber mold having a size of 180 × 25 × 25 mm, and vibration was applied for 1 hour to set the reinforcing material and settle. After molding, the entire rubber mold was cooled to -25 ° C, frozen, and demolded. After demolding, drying at 80 ° C. for 24 hours, firing at 450 ° C. for 5 hours in an air atmosphere at a heating rate of 50 ° C./h, and cooling to room temperature at a cooling rate of 50 ° C./h to perform a preform Was prepared. An Al-5Mg alloy having the same weight as the preform was placed on the obtained preform, and the alloy was impregnated with the alloy in a nitrogen gas stream at 825 ° C. (20 l / min: furnace volume 0.40 m 3 ). After that, cooling was performed in the same manner as in Example 1 to produce a metal-ceramic composite material.
【００３５】（２）評価 得られたプリフォームの粉末充填率、複合材料の曲げ強
度、破壊靱性値を実施例１と同様に求めた。それらの結
果を表２に示す。(2) Evaluation The powder filling rate of the obtained preform, the bending strength of the composite material, and the fracture toughness were determined in the same manner as in Example 1. Table 2 shows the results.
【００３６】（実施例５） （１）金属−セラミックス複合材料の作製 平均粒径が２０μｍの表面にシリカをコーティングした
ＡｌＮ粉末に対し、イオン交換水を２４ｗｔ％、固形分
濃度が２０％のコロイダルシリカ液（コロイドの大きさ
は１０×２０ｎｍ）を９．６ｗｔ％加え、ボールを入れ
てないポットミルで２時間混合した。得られたスラリー
を１８０×２５×２５ｍｍの大きさのシリコーンゴム型
に流し込み、１時間振動を印加して強化材を沈降させ成
形した。成形後、ゴム型ごと−２５℃に冷却し冷凍して
脱型した。脱型後、８０℃で２４時間乾燥した後、５０
℃／ｈの昇温速度で大気雰囲気中で７００℃で３時間焼
成した後、５０℃／ｈの降温速度で室温まで冷却してプ
リフォームを作製した。得られたプリフォームの上にプ
リフォームと同重量のＡｌ−２Ｍｇの合金を載置し、８
５０℃窒素気流中（２０リットル／ｍｉｎ：炉内容積
０．４０ｍ3）でプリフォームに合金を含浸させた後、
実施例１と同様に冷却して金属−セラミックスの複合材
料を作製した。Example 5 (1) Preparation of Metal-Ceramic Composite Material Colloidal having ion exchanged water of 24 wt% and solid content of 20% with respect to AlN powder having an average particle diameter of 20 μm coated with silica. 9.6 wt% of a silica liquid (colloid size: 10 × 20 nm) was added and mixed for 2 hours in a pot mill without balls. The obtained slurry was poured into a silicone rubber mold having a size of 180 × 25 × 25 mm, and vibration was applied for 1 hour to set the reinforcing material and settle. After molding, the entire rubber mold was cooled to -25 ° C, frozen, and demolded. After demolding and drying at 80 ° C. for 24 hours, 50
After sintering at 700 ° C. for 3 hours in an air atmosphere at a temperature rising rate of 50 ° C./h, it was cooled to room temperature at a temperature decreasing rate of 50 ° C./h to prepare a preform. An Al-2Mg alloy having the same weight as the preform was placed on the obtained preform, and 8
After the preform was impregnated with the alloy in a nitrogen stream at 50 ° C. (20 l / min: furnace volume 0.40 m 3 ),
Cooling was performed in the same manner as in Example 1 to produce a metal-ceramic composite material.
【００３７】（２）評価 得られたプリフォームの粉末充填率、複合材料の曲げ強
度、破壊靱性値を実施例１と同様に求めた。それらの結
果も表２に示す。(2) Evaluation The powder filling rate of the obtained preform, the bending strength of the composite material, and the fracture toughness were determined in the same manner as in Example 1. The results are also shown in Table 2.
【００３８】（実施例６） （１）金属−セラミックス複合材料の作製 平均粒径が２０μｍの表面にシリカをコーティングした
ＡｌＮ粉末に対し、イオン交換水を２４ｗｔ％、固形分
濃度が２０％のアルミナ水和物のコロイド液（コロイド
の大きさは１０×２０ｎｍ）を１０ｗｔ％加え、ボール
を入れてないポットミルで２時間混合した。得られたス
ラリーをφ２５０×ｔ１５ｍｍの大きさのシリコーンゴ
ム型に流し込み、１時間振動を印加して強化材を沈降さ
せ成形した。成形後、ゴム型ごと−２５℃に冷却し冷凍
して脱型した。脱型後、８０℃で２４時間乾燥した後、
５０℃／ｈの昇温速度で大気雰囲気中で４５０℃で５時
間焼成した後、５０℃／ｈの降温速度で室温まで冷却し
てプリフォームを作製した。得られたプリフォームの上
にプリフォームと同重量のＡｌ−５Ｍｇの合金を載置
し、８２５℃窒素気流中（２０リットル／ｍｉｎ：炉内
容積０．４０ｍ3）でプリフォームに合金を含浸させた
後、実施例１と同様に冷却して金属−セラミックスの複
合材料を作製した。Example 6 (1) Preparation of Metal-Ceramic Composite Material An AlN powder having an average particle diameter of 20 μm coated with silica was mixed with 24 wt% of ion-exchanged water and alumina having a solid concentration of 20%. A hydrate colloid solution (colloid size: 10 × 20 nm) was added at 10 wt%, and mixed for 2 hours in a pot mill without a ball. The obtained slurry was poured into a silicone rubber mold having a size of φ250 × t15 mm, and vibration was applied for one hour to set the reinforcing material and settle. After molding, the entire rubber mold was cooled to -25 ° C, frozen, and demolded. After demolding, after drying at 80 ° C for 24 hours,
After calcining at 450 ° C. for 5 hours in an air atmosphere at a temperature rising rate of 50 ° C./h, it was cooled to room temperature at a temperature decreasing rate of 50 ° C./h to prepare a preform. An Al-5Mg alloy having the same weight as the preform was placed on the obtained preform, and the alloy was impregnated with the alloy in a nitrogen gas stream at 825 ° C. (20 l / min: furnace volume 0.40 m 3 ). After that, cooling was performed in the same manner as in Example 1 to produce a metal-ceramic composite material.
【００３９】（２）評価 得られたプリフォームの粉末充填率、複合材料の曲げ強
度、破壊靱性値を実施例１と同様に求めた。それらの結
果も表２に示す。(2) Evaluation The powder filling rate of the obtained preform, the bending strength of the composite material, and the fracture toughness were determined in the same manner as in Example 1. The results are also shown in Table 2.
【００４０】（比較例２） （１）金属−セラミックス複合材料の作製 ５０×５０×１０ｍｍの金型に、平均粒径が１６μｍの
シリカをコーティングしたＡｌＮ粉末にポリカルボシラ
ン等の熱硬化性樹脂を５ｗｔ％加えて混合した粉末を充
填し、その粉末に２００℃で２トンの荷重を１時間加え
て成形し、その成形体を５０℃の昇温速度で空気中で７
００℃で５時間焼成しプリフォームを作製した。得られ
たプリフォームの上にプリフォームと同等量のＡｌ−５
Ｍｇの合金を載置し、８２５℃窒素気流中（２０リット
ル／ｍｉｎ：炉内容積０．４０ｍ3）でプリフォームに
合金を含浸させた後、実施例１と同様に冷却して金属−
セラミックスの複合材料を作製した。Comparative Example 2 (1) Preparation of Metal-Ceramic Composite Material Thermosetting resin such as polycarbosilane was applied to AlN powder obtained by coating a 50 × 50 × 10 mm mold with silica having an average particle size of 16 μm. Was added at 5 wt% and mixed, and the powder was molded by applying a load of 2 tons at 200 ° C. for 1 hour.
It was baked at 00 ° C. for 5 hours to prepare a preform. The same amount of Al-5 as the preform is placed on the obtained preform.
A Mg alloy was placed, and the preform was impregnated with the alloy in a nitrogen stream at 825 ° C. (20 l / min: furnace volume 0.40 m 3 ).
A composite material of ceramics was prepared.
【００４１】（２）評価 得られたプリフォームの粉末充填率、複合材料の曲げ強
度、破壊靱性値を実施例１と同様に求めた。それらの結
果も表２に示す。(2) Evaluation The powder filling rate of the obtained preform, the bending strength of the composite material, and the fracture toughness were determined in the same manner as in Example 1. The results are also shown in Table 2.
【００４２】（比較例３）シリカをコーティングしてな
いＡｌＮ粉末を用いた他は、実施例１と同様に金属−セ
ラミックス複合材料を作製し、同様に評価した。それら
の結果も表２に示す。Comparative Example 3 A metal-ceramic composite material was prepared and evaluated in the same manner as in Example 1, except that AlN powder not coated with silica was used. The results are also shown in Table 2.
【００４３】[0043]
【表１】 [Table 1]
【００４４】[0044]
【表２】 [Table 2]
【００４５】表１から明らかなように、水を用いないで
プリフォームを形成した実施例１〜３においては、プリ
フォームの形成がＡｌＮ粉末を容器に充填するだけであ
るので、いずれも粉末充填率が６０ｖｏｌ％より低く、
従来の粉末充填率を有する比較例１と同レベルのものし
か得られなかったが、その曲げ強度、破壊靱性値は、比
較例１よりいずれも高く、特性については従来よりかな
り向上していた。As is clear from Table 1, in Examples 1 to 3 in which preforms were formed without using water, the preforms were formed only by filling AlN powder into a container. The rate is lower than 60 vol%,
Although only the same level as that of Comparative Example 1 having the conventional powder filling rate was obtained, the flexural strength and fracture toughness were higher than those of Comparative Example 1, and the properties were considerably improved as compared with the conventional example.
【００４６】また、表２から明らかなように、実施例４
〜６においては、水を用い粉末をバインダーで結合させ
てプリフォームを形成しているので、従来の方法で作製
した比較例２の粉末充填率よりいずれも高く、しかもい
ずれも６０ｖｏｌ％を超えていた。これは、従来なし得
なかった粉末充填率が６０ｖｏｌ％を超えるＡｌＮ粉末
を強化材とした複合材料を容易に作製できることを示し
ている。そして、その曲げ強度、破壊靱性値とも比較例
２より低いものの、本発明と同じ方法でかつ同じ条件で
作製した他の強化材、例えば同レベルの粉末充填率を有
するＳｉＣ粉末で強化した複合材料と同等の強度を示し
ており、これは、耐水処理したＡｌＮ粉末でも耐水性の
ある他の粉末と同様に問題なく複合材料を作製できるこ
とを示している。なお、比較例３は、ＡｌＮ粉末に耐水
処理していないため、混合中水と反応して成形できなか
った。As is clear from Table 2, Example 4
In Nos. 6 to 6, since the preform was formed by bonding the powder with water using a binder, the powder filling ratio was higher than that of Comparative Example 2 produced by the conventional method, and all exceeded 60 vol%. Was. This indicates that a composite material using an AlN powder having a powder filling rate exceeding 60 vol%, which could not be obtained before, as a reinforcing material can be easily produced. And although its bending strength and fracture toughness value are both lower than Comparative Example 2, a composite material reinforced with another reinforcing material produced by the same method and under the same conditions as the present invention, for example, SiC powder having the same level of powder filling factor This indicates that the composite material can be produced without any problem, similarly to other water-resistant powders, even with the water-resistant AlN powder. In Comparative Example 3, since the AlN powder was not subjected to the water-resistant treatment, it could not be molded by reacting with water during mixing.
【００４７】さらに、上記実施例１、２、３、４、６の
プリフォームの大きさ、もしくは形状がいずれも異なっ
ていることから、またプレスでプリフォームを形成した
比較例１、２よりいずれも大きいものを作製してことか
ら、本発明では種々の形状品を、しかも大型品であって
も安価で容易に作製できることを示している。Further, since the sizes or shapes of the preforms of Examples 1, 2, 3, 4, and 6 were all different from each other, the comparative examples 1 and 2 in which the preforms were formed by pressing were all different. The present invention shows that various shaped articles can be easily manufactured at low cost even if the article is large in size.
【００４８】[0048]
【発明の効果】以上の通り、本発明の方法で金属−セラ
ミックス複合材料を作製すれば、ＡｌＮ粉末を用いて
も、含浸法で安価でしかも高い粉末充填率を有した金属
−セラミックス複合材料を容易に製造できるようになっ
た。このことにより、ＡｌＮは耐プラズマ性、高熱伝導
性に優れているので、これらの特性を生かした曲げ強
度、破壊靱性に優れた大型品を含むアルミニウム−Ａｌ
Ｎ複合材料を低コストで作製できるようになった。As described above, if a metal-ceramic composite material is produced by the method of the present invention, even if an AlN powder is used, a metal-ceramic composite material which is inexpensive and has a high powder filling rate by an impregnation method. It can be easily manufactured. As a result, AlN is excellent in plasma resistance and high thermal conductivity. Therefore, aluminum-Al including large-sized products excellent in bending strength and fracture toughness utilizing these characteristics is used.
N-composite materials can be produced at low cost.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 高橋 平四郎 千葉県松戸市松戸新田314−１ (72)発明者 林 睦夫 埼玉県浦和市大牧560 ──────────────────────────────────────────────────続 き Continuing on the front page (72) Inventor Heishiro Takahashi 314-1 Matsudo Nitta, Matsudo City, Chiba Prefecture (72) Mutsui Hayashi 560 Omaki, Urawa City, Saitama Prefecture
Claims (2)
してプリフォームを形成し、そのプリフォームに基材で
ある金属を含浸させる金属−セラミックス複合材料の製
造方法において、該プリフォームが、１〜１００μｍの
平均粒径を有し、３０〜６０ｖｏｌ％の粉末充填率を有
するＡｌＮ粉末から成り、該プリフォームの形成方法
が、ＡｌＮ粉末をカーボン等の容器中に充填して形成す
る方法であるとし、その形成されたプリフォームにアル
ミニウムを主成分とする合金を７００〜１０００℃の温
度で含浸させることを特徴とする金属−セラミックス複
合材料の製造方法。1. A method for producing a metal-ceramic composite material in which a preform is formed by using ceramic fibers or particles as a reinforcing material, and the preform is impregnated with a metal as a base material, wherein the preform has a size of 1 to 100 μm. The preform is formed of AlN powder having an average particle size and a powder filling rate of 30 to 60 vol%, and the method of forming the preform is a method of filling AlN powder into a container such as carbon to form the preform. A method for producing a metal-ceramic composite material, comprising: impregnating a formed preform with an alloy containing aluminum as a main component at a temperature of 700 to 1000 ° C.
してプリフォームを形成し、そのプリフォームに基材で
ある金属を含浸させる金属−セラミックス複合材料の製
造方法において、該プリフォームが、１〜１００μｍの
平均粒径を有し、６０〜８０ｖｏｌ％の粉末充填率を有
する耐水処理を施したＡｌＮ粉末から成り、該プリフォ
ームの形成方法が、ＡｌＮ粉末にコロイダルシリカ液ま
たは／及びアルミナ水和物のコロイド液を加え成形した
後、その成形体を焼成する方法であるとし、その形成さ
れたプリフォームにアルミニウムを主成分とする合金を
７００〜１０００℃の温度で含浸させることを特徴とす
る金属−セラミックス複合材料の製造方法。2. A method for producing a metal-ceramic composite material in which a preform is formed using ceramic fibers or particles as a reinforcing material, and the preform is impregnated with a metal as a base material, wherein the preform has a size of 1 to 100 μm. The preform is formed of a water-resistant AlN powder having an average particle size and a powder filling rate of 60 to 80 vol%, and the method of forming the preform is performed by adding a colloidal silica liquid or a colloid of alumina hydrate to the AlN powder. A metal-ceramics method, wherein the formed body is fired after adding a liquid, and the formed preform is impregnated with an alloy mainly composed of aluminum at a temperature of 700 to 1000 ° C. Manufacturing method of composite material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP30996096A JP4217279B2 (en) | 1996-11-07 | 1996-11-07 | Method for producing metal-ceramic composite material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP30996096A JP4217279B2 (en) | 1996-11-07 | 1996-11-07 | Method for producing metal-ceramic composite material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH10140262A true JPH10140262A (en) | 1998-05-26 |
| JP4217279B2 JP4217279B2 (en) | 2009-01-28 |
Family
ID=17999441
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP30996096A Expired - Fee Related JP4217279B2 (en) | 1996-11-07 | 1996-11-07 | Method for producing metal-ceramic composite material |
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| Country | Link |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008038171A (en) * | 2006-08-03 | 2008-02-21 | Aia Engineering Ltd | Improved wear-resistant metallic part and its manufacturing method |
| JP2010007149A (en) * | 2008-06-30 | 2010-01-14 | Taiheiyo Cement Corp | Metal matrix composite material |
-
1996
- 1996-11-07 JP JP30996096A patent/JP4217279B2/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008038171A (en) * | 2006-08-03 | 2008-02-21 | Aia Engineering Ltd | Improved wear-resistant metallic part and its manufacturing method |
| JP2010007149A (en) * | 2008-06-30 | 2010-01-14 | Taiheiyo Cement Corp | Metal matrix composite material |
Also Published As
| Publication number | Publication date |
|---|---|
| JP4217279B2 (en) | 2009-01-28 |
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