KR0183083B1 - Process for the preparation of molding of whiskers using complex materials - Google Patents

Process for the preparation of molding of whiskers using complex materials Download PDF

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KR0183083B1
KR0183083B1 KR1019940011723A KR19940011723A KR0183083B1 KR 0183083 B1 KR0183083 B1 KR 0183083B1 KR 1019940011723 A KR1019940011723 A KR 1019940011723A KR 19940011723 A KR19940011723 A KR 19940011723A KR 0183083 B1 KR0183083 B1 KR 0183083B1
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whisker
preform
aminopropyltrimethoxysilane
wet
cake
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KR1019940011723A
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KR950031973A (en
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안승균
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전성원
현대자동차주식회사
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/0072—Heat treatment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B28—WORKING CEMENT, CLAY, OR STONE
    • B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B1/00—Producing shaped prefabricated articles from the material
    • B28B1/26—Producing shaped prefabricated articles from the material by slip-casting, i.e. by casting a suspension or dispersion of the material in a liquid-absorbent or porous mould, the liquid being allowed to soak into or pass through the walls of the mould; Moulds therefor ; specially for manufacturing articles starting from a ceramic slip; Moulds therefor
    • B28B1/265—Producing shaped prefabricated articles from the material by slip-casting, i.e. by casting a suspension or dispersion of the material in a liquid-absorbent or porous mould, the liquid being allowed to soak into or pass through the walls of the mould; Moulds therefor ; specially for manufacturing articles starting from a ceramic slip; Moulds therefor pressure being applied on the slip in the filled mould or on the moulded article in the mould, e.g. pneumatically, by compressing slip in a closed mould
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/632—Organic additives
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/62227—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Structural Engineering (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Manufacture Of Alloys Or Alloy Compounds (AREA)
  • Reinforced Plastic Materials (AREA)
  • Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)

Abstract

휘스커 성분들 사이의 결합력이 강하고 복합화 기능이 향상된 휘스커 예비 성형체의 제조방법에 관한 것으로서, 휘스커 생성물을 γ-아미노프로필트리메톡시실란과 메탄올로 구성된 결합제 용액 내에 균질 분산시키고, 균질 분산액을 여과 및 탈수시켜 습윤 휘스커 케이크을 얻고, 습윤 휘스커 케이크을 금형에 주입하고 가압 성형하여 예비 성형체를 제작하고, 이를 400℃ 이상의 온도에서 약 30분간 가열하는 것으로 이루어지는 휘스커 예비 성형체의 제조방법.A method for producing a whisker preform having a strong binding force between the whisker components and an improved compounding function, wherein the whisker product is homogeneously dispersed in a binder solution composed of γ-aminopropyltrimethoxysilane and methanol, and the homogeneous dispersion is filtered and dehydrated. To obtain a wet whisker cake, inject the wet whisker cake into a mold and press molding to produce a preform, and heat it at a temperature of 400 ° C. or higher for about 30 minutes.

Description

[발명의 명칭][Name of invention]

복합재료용 휘스커 예비 성형체의 제조방법Manufacturing method of whisker preform for composite material

본 발명은 복합재료용 휘스커 예비 성형체의 제조방법에 관한 것으로서, 더욱 상세하게는 휘스커 성분들 사이의 결합력이 강하고 복합화 기능이 향상된 휘스커 예비 성형체의 제조방법에 관한 것이다.The present invention relates to a method for manufacturing a whisker preform for a composite material, and more particularly, to a method for manufacturing a whisker preform having a strong bonding force between whisker components and an improved compounding function.

종래에는 휘스커 예비 성형체의 제조방법으로서, 예를 들어 일분국 특개소 57-226545호에 개시된 바와 같이 휘스커 생성물을 물 또는 유기용매에 분산시켜 상압 또는 가압 하에서 여과시켜 형성시킨 습윤 휘스커 케이크을 소정밀도가 되게 압축한 후 건조처리하는 방법이 사용되어 왔다. 그러나 이 방법으로 제조된 예비 성형체는 결합력이 낮은 문제점이 있다.Conventionally, as a method for producing a whisker preform, a wet whisker cake formed by dispersing a whisker product in water or an organic solvent and filtering under normal pressure or pressure, as disclosed in Japanese Patent Application Laid-Open No. 57-226545, to a predetermined density, for example. The method of compressing and then drying has been used. However, the preform manufactured by this method has a problem of low binding force.

또한 일본국 특개소 60-49292호에는 휘스커 성분들 사이의 결합력을 강화하기 위하여 휘스커 생성물을 실란 커플링제를 함유하는 용액 중에 분산시킨 후 여과 형성시킨 습윤 휘스커 케이크을 건조처리하는 방법이 개시되어 있다. 이 방법에서는 예비성형체에 액상의 매트릭스 금속을 침투시킬 때 예비 성형체 내 실란 커플링제 중의 탄소원자가 분해되어 나와 탄화물(carbide)을 형성하므로써 복합화 기능히 약화되는 단점이 있다. 또한 매트릭스 금속 침투시에 예비 성형체의 변형을 일으키는 문제점이 있다.In addition, Japanese Patent Application Laid-Open No. 60-49292 discloses a method of drying a wet whisker cake formed by dispersing a whisker product in a solution containing a silane coupling agent and then filtrating to enhance the binding force between the whisker components. In this method, when the liquid matrix metal is penetrated into the preform, the carbon atom in the silane coupling agent in the preform is decomposed to form a carbide, thereby weakening the compounding function. In addition, there is a problem of causing deformation of the preform when the matrix metal penetrates.

본 발명은 상기한 바와 같은 종래기술의 문제점을 해결하기 위한 것으로서, 휘스커 성분들 사이의 결합력이 강하고 복합화 기능이 향상되며 매트릭스 금속 침투시의 변형이 최소화된 휘스커 예비 성형체를 제공함을 목적으로 한다.The present invention is to solve the problems of the prior art as described above, an object of the present invention is to provide a whisker preform having a strong binding force between the whisker components, improved compounding function and minimized deformation during matrix metal penetration.

상기한 목적을 달성하기 위하여 본 발명은, 휘스커 생성물을 γ-아미노프로필트리메톡시실란과 메탄올로 구성된 결합제 용액에 균질 분산시키고, 균질 분산액을 여과 및 탈수시켜 습윤 휘스커 케이크을 얻고, 습윤휘스커 케이크을 금형에 주입하고 가압성형하여 예비 성형체를 얻고, 이를 400℃ 이상의 온도에서 약 30분간 가열하는 것으로 이루어지는 휘스커 예비 성형체의 제조방법을 제공한다.In order to achieve the above object, the present invention is to homogeneously disperse the whisker product in a binder solution consisting of γ-aminopropyltrimethoxysilane and methanol, and to filter and dehydrate the homogeneous dispersion to obtain a wet whisker cake, the wet whisker cake into a mold Provided is a method for producing a whisker preform consisting of injection and pressing to obtain a preform, which is heated at a temperature of 400 ° C. or higher for about 30 minutes.

본 발명을 상세히 설명하면 다음과 같다.The present invention is described in detail as follows.

결합제로서 사용되는 γ-아미노프로필트리메톡시실란은 하기 일반식을 갖는다.Γ-aminopropyltrimethoxysilane used as the binder has the following general formula.

γ-NH2(CH2)3Si(OCH3)3 γ-NH 2 (CH 2 ) 3 Si (OCH 3 ) 3

상기 일반식으로 나타내어지는 γ-아미노프로필트리메톡시실란은 다음과 같은 특징이 있다.Γ-aminopropyltrimethoxysilane represented by the above general formula has the following characteristics.

① 동일 분자 중에 유기상 및 무기상에 서로 반응하여 화학적 결합을 하는 2종류의 반응기, 즉 메틸기와 아미노기를 함유한다.(1) It contains two kinds of reactors which react with each other in an organic phase and an inorganic phase in the same molecule to form a chemical bond, that is, methyl and amino groups.

② 가열시에 열분해 반응을 일으켜 실란 화합물이 Si 원자와 O 원자의 강고한 결합을 유지하게 된다.② Pyrolysis reaction occurs at the time of heating, and the silane compound maintains a strong bond between Si and O atoms.

이상과 같은 특징으로 인하여 γ-아미노프로필트리메톡시실란을 결합제로 사용하는 경우에, 강한 결합력을 갖는 휘스커 예비 성형체가 제조되며 따라서 금속 침투시에 예비 성형체의 변형이 최소화될 수 있다.Due to the above characteristics, when γ-aminopropyltrimethoxysilane is used as a binder, a whisker preform having a strong binding force is produced, and thus deformation of the preform can be minimized during metal penetration.

결합제 용액을 구성하는 γ-아미노프로필트리메톡시실란과 메탄올의 비율은 결합제 용액 내 γ-아미노프로필트리메톡시실란의 농도가 3 내지 5 중량% 범위내인 것이 바람직하다. 상기 농도가 3 중량% 미만인 경우에는 계면 결합 효과가 낮고, 5 중량% 초과시에는 매트릭스 금속의 침투가 곤란해지는 문제점이 발생한다.The ratio of γ-aminopropyltrimethoxysilane and methanol constituting the binder solution is preferably in the range of 3 to 5% by weight of γ-aminopropyltrimethoxysilane in the binder solution. If the concentration is less than 3% by weight, the interfacial bonding effect is low, and when the concentration is more than 5% by weight, it is difficult to penetrate the matrix metal.

휘스커 생성물과 결합제 용액의 사용비는 중량비로 1 : 9.5 내지 1 : 10.5 범위내가 적당하며 1 : 10이 바람직하다.The use ratio of the whisker product and the binder solution is suitably in the range of 1: 9.5 to 1: 10.5 by weight, and preferably 1:10.

습윤 휘스커 케이크을 가압 성형하는 단계에서는 최종 예비 성형체의 부피비율, 형상을 고려하여 가압 성형한다.In the step of press molding the wet whisker cake, pressure molding is performed in consideration of the volume ratio and the shape of the final preform.

성형하여 얻은 휘스커 예비 성형체를 400℃ 이상 온도, 바람직하게는 400 내지 450℃ 온도에서 약 30분간 가열하는데, 이는 탄소원자를 복합화 공정 이전에 기체화시켜 휘발 제거하기 위하여 실시한다.The whisker preform obtained by molding is heated at a temperature of 400 ° C. or higher, preferably 400 to 450 ° C. for about 30 minutes, which is carried out to volatilize and remove carbon atoms prior to the compounding process.

최종적으로 얻어진 휘스커 예비 성형체는의 강고한 결합력을 갖는다.The final whisker preform obtained Has a strong bonding force.

하기에 본 발명의 바람직한 실시예를 기재하여 더욱 상세히 설명하기로 한다.Hereinafter, the preferred embodiments of the present invention will be described in more detail.

[실시예]EXAMPLE

휘스커 생성물 100g을 3중량% γ-아미노프로필트리메톡시실란의 메탄올 용액(3중량% γ-아미노프로필트리메톡시실란+97% 메탄올) 내에 균질화기(homogenizer)를 이용하여 분산시켰다. 얻어진 분산액을 진공여과장치에 주입하여 여과시킨 후, 여과 필터 위에 남은 습윤 휘스커 케이크을 금형내에 주입하고 5kg/㎠ 압력하에 가압성형하여 예비성형체를 제조하였다. 이 예비 성형체를 400℃의 오븐 내에서 약 30분간 가열하여 최종 휘스커 예비 성형체를 수득하였다.100 g of whisker product was dispersed using a homogenizer in a methanol solution of 3% by weight γ-aminopropyltrimethoxysilane (3% by weight γ-aminopropyltrimethoxysilane + 97% methanol). After the obtained dispersion was injected into a vacuum filtration apparatus and filtered, the wet whisker cake remaining on the filtration filter was injected into the mold and press-molded under a pressure of 5 kg / cm 2 to prepare a preform. This preform was heated in an oven at 400 ° C. for about 30 minutes to obtain a final whisker preform.

[비교예][Comparative Example]

휘스커 생성물 100g을 3중량% γ-아미노프로필트리메톡시실란의 메탄올 용액(3중량% γ-아미노프로필트리메톡시실란+97% 메탄올) 내에 균질화기(homogenizer)를 이용하여 분산시켰다. 얻어진 분산액을 진공 여과장치에 주입하여 여과시킨 후, 여과 필터 위에 남은 습윤 휘스커 케이크을 금형내에 주입하고 5kg/㎠ 압력하에 가압성형하여 예비성형체를 제조하였다.100 g of whisker product was dispersed using a homogenizer in a methanol solution of 3% by weight γ-aminopropyltrimethoxysilane (3% by weight γ-aminopropyltrimethoxysilane + 97% methanol). After the obtained dispersion was injected into a vacuum filtration apparatus and filtered, the wet whisker cake remaining on the filtration filter was injected into the mold and press-molded under a pressure of 5 kg / cm 2 to prepare a preform.

이 예비 성형체를 자연 건조시킨 후 120℃에서 건조하여 최종 휘스커 예비 성형체를 습득하였다.The preform was naturally dried and then dried at 120 ° C. to obtain a final whisker preform.

상기 실시예 및 비교예에서 얻어진 최종 휘스커 예비 성형체(30×10×100)를 스팬거리 700mm로 하여 굴곡 강도 시험을 행하여 그 결과를 다음의 표 1에 나타내었다.The final whisker preforms (30 × 10 × 100) obtained in Examples and Comparative Examples were subjected to flexural strength testing with a span distance of 700 mm, and the results are shown in Table 1 below.

표1에서 보듯이 본 발명에 따라 제조되어지는 휘스커 예비 성형체는 높은 굴곡 강도를 갖는 우수한 물성을 갖음을 알 수 있다.As shown in Table 1, it can be seen that the whisker preform manufactured according to the present invention has excellent physical properties with high flexural strength.

Claims (4)

휘스커 생성물을 γ-아미노프로필트리메톡시실란과 메탄올로 구성된 결합제 용액 내에 균질 분산시키고, 균질 분산액을 여과 및 탈수시켜 습윤 휘스커 케익을 얻고, 습윤 휘스커 케익을 금형에 주입하고 가압 성형하여 예비 성형체를 제작하고, 이를 400℃ 이상의 온도에서 약 30분간 가열하는 것으로 이루어지는 휘스커 예비 성형체의 제조 방법.The whisker product is homogeneously dispersed in a binder solution consisting of γ-aminopropyltrimethoxysilane and methanol, the homogeneous dispersion is filtered and dehydrated to obtain a wet whisker cake, the wet whisker cake is injected into a mold and pressure molded to form a preform. And heating it at a temperature of 400 ° C or higher for about 30 minutes. 제1항에 있어서, 결합제 용액내에서 γ-아미노프로필트리메톡시실란의 농도는3 내지 5 중량% 임을 특징으로 하는 방법.The method of claim 1, wherein the concentration of γ-aminopropyltrimethoxysilane in the binder solution is 3 to 5% by weight. 제1항에 있어서, 휘스커 생성물과 결합제 용액의 사용비는 1:9.5 내지 1:10.5 범위내인 것을 특징으로 하는 방법.The method of claim 1 wherein the ratio of whisker product and binder solution is in the range of 1: 9.5 to 1: 10.5. 제1항에 있어서, 가압 성형하여 제조된 예비성형체를 400℃ 내지 450℃ 온도에서 가열하는 것을 특징으로 하는 방법.The method of claim 1, wherein the preform produced by pressure molding is heated at a temperature of 400 ℃ to 450 ℃.
KR1019940011723A 1994-05-28 1994-05-28 Process for the preparation of molding of whiskers using complex materials KR0183083B1 (en)

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