JPS6410582B2 - - Google Patents
Info
- Publication number
- JPS6410582B2 JPS6410582B2 JP22274885A JP22274885A JPS6410582B2 JP S6410582 B2 JPS6410582 B2 JP S6410582B2 JP 22274885 A JP22274885 A JP 22274885A JP 22274885 A JP22274885 A JP 22274885A JP S6410582 B2 JPS6410582 B2 JP S6410582B2
- Authority
- JP
- Japan
- Prior art keywords
- whisker
- preform
- silane coupling
- coupling agent
- whiskers
- 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.)
- Expired
Links
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000000243 solution Substances 0.000 description 7
- 239000011159 matrix material Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 239000002905 metal composite material Substances 0.000 description 5
- 210000002808 connective tissue Anatomy 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000000805 composite resin Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000003733 fiber-reinforced composite Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 125000004430 oxygen atom Chemical group O* 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000005979 thermal decomposition reaction Methods 0.000 description 2
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 1
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- OBNDGIHQAIXEAO-UHFFFAOYSA-N [O].[Si] Chemical group [O].[Si] OBNDGIHQAIXEAO-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000002144 chemical decomposition reaction Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000002542 deteriorative effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 125000005395 methacrylic acid group Chemical group 0.000 description 1
- -1 methoxy, ethoxy Chemical group 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 150000004756 silanes Chemical class 0.000 description 1
- 125000005372 silanol group Chemical group 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 210000001519 tissue Anatomy 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Reinforced Plastic Materials (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Manufacture Of Alloys Or Alloy Compounds (AREA)
Description
「産業上の利用分野」
本発明は、液状のマトリツクス物質を溶浸ある
いは含浸して繊維強化複合材を製造する際に、そ
の繊維質骨格として用いるウイスカープリフオー
ム強化形成方法に関する。
「従来の技術」
SiCウイスカー、Si3N4ウイスカーなどを強化
材として繊維強化複合材を製造する方法の１つに
ウイスカー集合体から成るプリフオームを形成
し、このプリフオームに液状のマトリツクス物質
を圧入固化させる方法がある。この方法によつて
得られる複合材は、繊維質骨格となるウイスカー
プリフオームの性状に左右され、例えばウイスカ
ープリフオームの密度や組織構造の均質性などに
よつてその特性は大きく左右される。とくに、液
状のマトリツクス物質の圧入時にウイスカープリ
フオームが変形したり、亀裂を生じたりすること
なく原形を保持し得る程度の十分な強度を有する
ことが必要である。
出願人は、先に複合材用ウイスカープリフオー
ムを形成する効果的な手段としてウイスカー生成
物を水または有機溶媒に分散し、これを常圧また
は加圧下に過して残留する湿潤ウイスカーケー
キをそのまま、もしくは所定密度に圧縮した後、
乾燥処理する方法を提案した（特願昭57−
226545、同59−12049）。これら先行技術によるウ
イスカープリフオームは、ウイスカーのみの集合
体であるにもかかわらず極めて均質な一体的組織
構造を有している。しかし、強度的に充分でな
く、とくに低密度のプリフオームを形成する場合
には強度特性の低下が著しい。したがつて、マト
リツクス物質の圧入時に変形を生じ易く、複合材
の性能を劣化させる難点があつた。
この難点を排除し、ウイスカープリフオームの
強化をはかる方法として各種バインダーを含む溶
液中に分散させる方法がある。この見地から、出
願人はウイスカーをシランカツプリング剤を含む
溶液中に分散させた後、過形成した湿潤ウイス
カーケーキを乾燥処理する方法を提案した（特願
昭60−49292）。この手法はプリフオームの強化が
はかられるばかりではなく、マトリツクス物質と
して樹脂を使用する場合には、樹脂との界面結合
機能が促進強化され、機械的強度特性のすぐれた
ウイスカー強化樹脂複合材を製造することができ
る。
「発明が解決しようとする問題点」
しかしながら、マトリツクス物質として金属を
使用し、ウイスカー強化金属複合材を製造する場
合には、プリフオーム中に生成したシランカツプ
リング剤相互の結合組織構造が圧入する高温の金
属溶湯により分解される。その結果、プリフオー
ムの強化機能が損われるばかりでなく、分解時に
発生するガスの一部が金属複合材中に残留してそ
の性能を劣化させ、さらにシランカツプリング剤
中の炭素原子によるカーバイドが生成するなどの
欠点があつた。
「問題点を解決するための手段」
本発明は、上記欠点のないウイスカープリフオ
ームの強化形成方法を提供するものである。
すなわち、本発明は生成ウイスカーをシランカ
ツプリング剤を含む溶液中に分散させた後、常圧
または加圧下に過して得られた湿潤ウイスカー
ケーキをそのままもしくは所定密度に圧縮して乾
燥し、次いで600℃以上の温度で熱処理すること
を構成的特徴とするウイスカープリフオームの強
化形成方法である。
ウイスカーとしては、SiCウイスカー、Si3N4
ウイスカーが用いられ、生成ウイスカーは直径
0.1〜5μｍ、長さ10〜500μｍの微細短繊維状の単
結晶が絡み合つた組織体を呈している。
シランカツプリング剤は、同一分子中に有機相
と無機相にそれぞれ反応し、化学的に結合する２
種類の異なつた反応基を有しいる。すなわち、無
機質と化学結合するメトキシ基、エトキシ基、シ
ラノール基などと有機質材料と化学結合するビニ
ル基、メタクリル基、アミノ基などの反応基を有
しており、界面に作用して化学的に両者を結合さ
せ、あるいは親和性を高め樹脂複合材の物性向上
にすぐれた機能を発揮する。
本発明は、シランカツプリング剤の有するこの
結合機能に着目し、さらに熱処理を施すことによ
り化学反応や熱分解反応を起生させてシラン化合
物相互の結合を、ケイ素原子と酸素原子の強固な
結合構造に転換するものである。
まず、生成ウイスカーをシランカツプリング剤
を含む溶液に入れて充分に撹拌混合し、均一な分
散液を調製する。この場合、シランカツプリング
剤の熱処理による界面結合機能を充分に付与する
ためには少なくとも１重量％以上の濃度が必要で
ある。しかし５重量％を越える濃度の溶液で処理
してもそれ以上の界面結合効果は認められない。
なお、シランカツプリング剤の溶液１に対しウ
イスカーを10〜100ｇの割合で混合すると、均一
分散液を調製するとともに処理能率の向上をはか
ることができ好ましい。撹拌混合は、インペラー
型や渦流型など通常使用される適宜な撹拌手段が
適用される。
このウイスカー分散液を過処理して湿潤ウイ
スカーケーキとし、これをそのままもしくは所定
密度に圧縮したのち乾燥処理することによつてウ
イスカープリフオームが形成される。このウイス
カープリフオームは、ウイスカーの表面に付着し
たシランカツプリング剤相互の結合を介して強化
形成されている。次に、このプリフオームを600
℃以上の温度で熱処理して化学反応や熱分解反応
によりシランカツプリング剤相互の結合を、ケイ
素原子と酸素原子の強固な結合組織構造
"Industrial Application Field" The present invention relates to a method for forming a reinforced whisker preform used as a fibrous skeleton when manufacturing a fiber-reinforced composite material by infiltrating or impregnating it with a liquid matrix material. "Conventional technology" One of the methods for manufacturing fiber reinforced composite materials using SiC whiskers, Si 3 N 4 whiskers, etc. as reinforcing materials is to form a preform consisting of a whisker aggregate, and then press a liquid matrix material into this preform and solidify it. There is a way to do it. The composite material obtained by this method depends on the properties of the whisker preform, which is the fibrous skeleton, and its properties are greatly affected by, for example, the density of the whisker preform and the homogeneity of the tissue structure. In particular, it is necessary that the whisker preform has sufficient strength to maintain its original shape without deforming or cracking when the liquid matrix material is press-fitted. The applicant first disperses the whisker product in water or an organic solvent as an effective means of forming a whisker preform for a composite material, and then passes this under normal pressure or pressurization to leave the remaining wet whisker cake as it is. , or after compressing to a predetermined density,
proposed a drying method (patent application 1982-
226545, 59-12049). Although these whisker preforms according to the prior art are aggregates of only whiskers, they have an extremely homogeneous integral structure. However, it is not strong enough, and particularly when forming a low-density preform, the strength characteristics are significantly deteriorated. Therefore, when the matrix material is press-fitted, deformation tends to occur, which has the disadvantage of deteriorating the performance of the composite material. One way to eliminate this difficulty and strengthen the whisker preform is to disperse it in a solution containing various binders. From this point of view, the applicant proposed a method of drying the overformed wet whisker cake after dispersing the whiskers in a solution containing a silane coupling agent (Japanese Patent Application No. 60-49292). This method not only strengthens the preform, but also promotes and strengthens the interfacial bonding function with the resin when resin is used as the matrix material, producing whisker-reinforced resin composites with excellent mechanical strength properties. can do. ``Problems to be Solved by the Invention'' However, when metal is used as the matrix material and whisker-reinforced metal composites are manufactured, high temperatures are required where the connective tissue structure of the silane coupling agent formed in the preform is press-fitted. Decomposed by molten metal. As a result, not only the strengthening function of the preform is impaired, but also some of the gases generated during decomposition remain in the metal composite and deteriorate its performance, and the carbon atoms in the silane coupling agent form carbides. There were drawbacks such as: ``Means for Solving the Problems'' The present invention provides a method for forming a reinforced whisker preform that does not have the above-mentioned drawbacks. That is, in the present invention, the produced whiskers are dispersed in a solution containing a silane coupling agent, and then the resulting wet whisker cake is dried as it is or compressed to a predetermined density by passing under normal pressure or pressurization. This is a method for forming a strengthened whisker preform that is structurally characterized by heat treatment at a temperature of 600°C or higher. As a whisker, SiC whisker, Si 3 N 4
Whiskers are used, and the generated whiskers have a diameter
It exhibits an intertwined structure of fine short fiber-like single crystals of 0.1 to 5 μm and 10 to 500 μm in length. A silane coupling agent is a silane coupling agent that reacts with the organic phase and inorganic phase in the same molecule and chemically bonds them.
It has different types of reactive groups. In other words, it has reactive groups such as methoxy, ethoxy, and silanol groups that chemically bond with inorganic materials, and vinyl groups, methacrylic groups, and amino groups that chemically bond with organic materials. It exhibits excellent functionality in improving the physical properties of resin composite materials by binding or increasing affinity. The present invention focuses on this bonding function of the silane coupling agent, and further heat-treats it to cause a chemical reaction or thermal decomposition reaction to strengthen the bonds between silane compounds and strengthen the strong bonds between silicon atoms and oxygen atoms. It is a transformation into structure. First, generated whiskers are placed in a solution containing a silane coupling agent and thoroughly stirred and mixed to prepare a uniform dispersion. In this case, the concentration of the silane coupling agent must be at least 1% by weight or more in order to provide sufficient interfacial bonding function through heat treatment. However, even when treated with a solution having a concentration exceeding 5% by weight, no further interfacial bonding effect is observed.
It is preferable to mix whiskers at a ratio of 10 to 100 g per 1 part of the silane coupling agent solution, since a uniform dispersion can be prepared and processing efficiency can be improved. For stirring and mixing, a commonly used appropriate stirring means such as an impeller type or a vortex type is applied. A whisker preform is formed by over-processing this whisker dispersion to form a wet whisker cake, which is then dried as it is or after being compressed to a predetermined density. This whisker preform is reinforced through mutual bonding of the silane coupling agent attached to the whisker surface. Next, set this preform to 600
The silane coupling agent is bonded to each other through chemical and thermal decomposition reactions through heat treatment at temperatures above ℃, creating a strong connective tissue structure of silicon atoms and oxygen atoms.
【式】に転換する。
「作用」
上記構成に基づき、ウイスカープリフオーム中
に均一に形成した薄膜状のシランカツプリング剤
相互の結合構造が、熱処理により高温に対して安
定強固な結合組織構造に転換される。
「実施例」
ケイ素源原料と炭材とを混合し、非酸化性雰囲
気下で1600℃の温度で反応させたのち、残留する
炭材成分を焼却除去して直径0.5〜1.5μｍ、長さ
10〜300μｍのβ型SiCウイスカーを生成した。こ
の生成SiCウイスカー300ｇをシランカツプリン
グ剤としてγ−アミノプロピルトリエトキシシラ
ン（信越化学(株)製KBE903）を用いエタノールを
溶媒として３％の溶液５中に均一に分散させ
た。この分散液を直径100mmの円筒状過装置に
注入し、５Kg／cm2の圧縮空気を圧入して加圧過
したのち乾燥処理して円柱状（直径100mm、高さ
100mm）のウイスカープリフオームを形成した。
次いで、このプリフオームを600℃の温度で１時
間熱処理したのち圧縮強度を測定して、その結果
を表−１に示した。表−１には比較例として、熱
処理を施さない場合の測定結果についても併記し
た。Convert to [formula]. "Operation" Based on the above structure, the bonding structure between the thin film-like silane coupling agents uniformly formed in the whisker preform is converted into a connective tissue structure that is stable and strong against high temperatures by heat treatment. "Example" A silicon source material and a carbonaceous material are mixed and reacted at a temperature of 1600℃ in a non-oxidizing atmosphere, and the remaining carbonaceous component is removed by incineration to obtain a material with a diameter of 0.5 to 1.5μm and a length of
β-type SiC whiskers of 10 to 300 μm were produced. 300 g of the produced SiC whiskers were uniformly dispersed in a 3% solution 5 using γ-aminopropyltriethoxysilane (KBE903, manufactured by Shin-Etsu Chemical Co., Ltd.) as a silane coupling agent and ethanol as a solvent. This dispersion was injected into a cylindrical filtration device with a diameter of 100 mm, and 5 kg/cm 2 of compressed air was injected to pressurize it, and then dried to form a cylindrical shape (diameter 100 mm, height
A whisker preform of 100mm) was formed.
Next, this preform was heat treated at a temperature of 600° C. for 1 hour, and then its compressive strength was measured, and the results are shown in Table 1. As a comparative example, Table 1 also shows the measurement results without heat treatment.
【表】
(注) ※ ８％圧縮歪における応力値
これらのプリフオームをモールド内にセツト
し、800℃に加熱溶融したAl合金（5052）を注湯
して1000Kg／cm2の加圧下に圧入した後冷却固化し
てウイスカー強化金属複合材を製造した。溶湯圧
入によるプリフオームの変形を複合化前後の高さ
の変化から算出して表−２に示した。また、表−
２には、得られた金属複合材の諸特性について測
定した結果についても記載した。[Table] (Note) * Stress value at 8% compressive strain These preforms were set in a mold, and Al alloy (5052) heated and melted at 800℃ was poured and press-fitted under a pressure of 1000Kg/cm 2 . After cooling and solidifying, a whisker-reinforced metal composite was produced. The deformation of the preform due to injection of molten metal was calculated from the change in height before and after compounding, and is shown in Table 2. Also, table -
2 also describes the results of measuring various properties of the obtained metal composite material.
【表】【table】
【表】
これらの結果から、発明例のプリフオームは高
温においても充分な強度を示し安定であるが、比
較例の場合には溶湯圧入時の高温によりシランカ
ツプリング剤が分解して強度が低下するとともに
分解ガスの吸蔵やカーバイドの生成により強度特
性の低下が認められる。
「発明の効果」
上記説明で明らかなように本発明は、シランカ
ツプリング剤相互の結合構造を熱処理することに
より、ケイ素−酸素原子の高温において安定性の
高い結合組織構造に転換するものである。その結
果、金属溶湯圧入時の高温にも耐えてプリフオー
ムの変形が少なく、機械的強度特性のすぐれたウ
イスカー強化金属複合材を製造することが可能と
なる。[Table] From these results, the preform of the invention example shows sufficient strength and is stable even at high temperatures, but in the case of the comparative example, the silane coupling agent decomposes due to the high temperature during injection of molten metal, resulting in a decrease in strength. At the same time, a decrease in strength properties is observed due to the absorption of cracked gas and the formation of carbide. "Effects of the Invention" As is clear from the above explanation, the present invention converts the bonding structure between the silane coupling agents into a connective tissue structure of silicon-oxygen atoms that is highly stable at high temperatures by heat-treating the structure. . As a result, it is possible to produce a whisker-reinforced metal composite material that can withstand high temperatures during injection of molten metal, has minimal deformation of the preform, and has excellent mechanical strength characteristics.
Claims (1)
む溶液中に分散させた後、常圧または加圧下に
過して得られた湿潤ウイスカーケーキをそのまま
もしくは所定密度に圧縮して乾燥し、次いで600
℃以上の温度で熱処理することを特徴とするウイ
スカープリフオームの強化形成方法。 ２ シランカツプリング剤の濃度が１〜５重量％
である特許請求の範囲第１項記載のウイスカープ
リフオームの強化形成方法。[Claims] 1. After dispersing the generated whiskers in a solution containing a silane coupling agent, the resulting wet whisker cake is dried as it is or after being compressed to a predetermined density. , then 600
A method for forming a strengthened whisker preform characterized by heat treatment at a temperature of ℃ or higher. 2 The concentration of the silane coupling agent is 1 to 5% by weight.
A method for forming a reinforced whisker preform according to claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP22274885A JPS6283439A (en) | 1985-10-08 | 1985-10-08 | Formation of whisker perform for reinforcement |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP22274885A JPS6283439A (en) | 1985-10-08 | 1985-10-08 | Formation of whisker perform for reinforcement |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6283439A JPS6283439A (en) | 1987-04-16 |
| JPS6410582B2 true JPS6410582B2 (en) | 1989-02-22 |
Family
ID=16787287
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP22274885A Granted JPS6283439A (en) | 1985-10-08 | 1985-10-08 | Formation of whisker perform for reinforcement |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6283439A (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6483632A (en) * | 1987-09-25 | 1989-03-29 | Ube Industries | Reinforcing fiber preform for metal-base composite material and its production |
-
1985
- 1985-10-08 JP JP22274885A patent/JPS6283439A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6283439A (en) | 1987-04-16 |
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