KR100213316B1 - Process for producing complex materials - Google Patents
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- KR100213316B1 KR100213316B1 KR1019950045337A KR19950045337A KR100213316B1 KR 100213316 B1 KR100213316 B1 KR 100213316B1 KR 1019950045337 A KR1019950045337 A KR 1019950045337A KR 19950045337 A KR19950045337 A KR 19950045337A KR 100213316 B1 KR100213316 B1 KR 100213316B1
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Abstract
수성 분산매질 및 바인더를 사용하지 않고 금속 복합재료 제조용 예비성형체를 제조하는 방법이 제공된다.A method is provided for producing a preform for the production of metal composite materials without the use of an aqueous dispersion medium and a binder.
세라믹 강화재를 실리콘 오일에 분산시킨 다음, 흡인여과, 건조 및 열처리 함으로써 실리콘 오일의 실리콘이 열처리 동안 대기중의 산소와 반응하여 SiO2를 형성하게 되고 이 SiO2형성에 의해 강화재로 이루어진 예비성형체의 강도를 얻을 수 있다.The ceramic reinforcing material is dispersed in the silicone oil, followed by suction filtration, drying and heat treatment, so that the silicon of the silicone oil reacts with oxygen in the air during the heat treatment to form SiO 2 , and the strength of the preform made of the reinforcing material is formed by the SiO 2 formation. Can be obtained.
물, 알콜등 수성 분산매질을 사용하는, 또한 강도 확보를 위해 무기질 바인더를 사용하던 종래의 방법에 비하여 공정이 간단할 뿐만 아니라 제조원가에도 기여할 수 있다.Compared to the conventional method using an aqueous dispersion medium such as water or alcohol and using an inorganic binder to secure strength, the process is simple and contributes to manufacturing cost.
Description
제1도는 종래의 예비성형체 제조방법을 도시한 공정 개략도.1 is a process schematic diagram showing a conventional method for producing a preform.
제2도는 통상의 예비성형체 제조장치의 개략 단면도.2 is a schematic cross-sectional view of a conventional preform manufacturing apparatus.
제3도는 본 발명에 의한 예비성형체 제조방법을 도시한 공정 개략도.3 is a process schematic diagram showing a method for producing a preform according to the present invention.
제4a도는 본 발명의 방법에 따라 제조된 예비성형체의 내부조직을 보여주는 주사전자 현미경 사진.Figure 4a is a scanning electron micrograph showing the internal structure of the preform prepared according to the method of the present invention.
b도는 종래방법에 따라 제조된 예비성형체의 내부조직을 보여주는 주사전자 현미경 사진.b is a scanning electron micrograph showing the internal structure of the preform prepared according to the conventional method.
* 도면의 주요부분에 대한 부호의 설명* Explanation of symbols for main parts of the drawings
1 : 본체 2 : 실리콘 오일 분산물1: Body 2: Silicone Oil Dispersion
3 : 세라믹강화재 4 : 필터3: ceramic reinforcing material 4: filter
5 : 배출구5: outlet
본 발명은 금속복합재료 제조용 예비성형체 제조방법에 관한 것이며, 보다 상세히는 금속복합재료 제조시 강화재로 사용되는 예비성형체를 바인더를 사용하지 않고 제조하는 방법에 관한 것이다.The present invention relates to a method for producing a preform for manufacturing a metal composite material, and more particularly, to a method for producing a preform used as a reinforcing material in the manufacture of a metal composite material without using a binder.
금속복합재료는 경량이면서 고강도 및 고강성을 가지고 있기 때문에 항공우주분야에 사용되는 소재로서 뿐만 아니라 자동차의 경량화를 위한 부품으로도 많이 사용되고 있다.Metal composite materials are lightweight, have high strength and high rigidity, so they are used not only as materials for aerospace, but also as components for weight reduction of automobiles.
즉, 금속 복합재료는 연질의 금속기지내에 단섬유, 휘스커, 입자등과 같은 경질의 세라믹 경화재를 분산시켜 제조하기 때문에 인장강도 및 탄성률등의 기계적 성질이 우수한 장점이 있는 것이다.That is, the metal composite material is produced by dispersing a hard ceramic cured material such as short fibers, whiskers, particles, etc. in a soft metal base, and thus has excellent mechanical properties such as tensile strength and elastic modulus.
이같은 금속 복합재료의 제조에 있어서는 금속과 세라믹 강화재를 혼합시 상호간의 젖음성이 좋지 않기 때문에 미리 세라믹 강화재로 예비성형체를 형성한 후 형성된 예비성형체에 금속을 용해하여 용탕단조법으로 기계적 압력을 가함으로써 예비성형체 내부에 금속을 침투시키는 방법이 주로 사용되고 있다(일본 공개특허 소63-128965 참조).In the preparation of such a metal composite material, when the metal and the ceramic reinforcing material are mixed with each other, the wettability of each other is not good. The method of making metal penetrate into a molded object is mainly used (refer Japanese Unexamined-Japanese-Patent No. 63-128965).
한편 상기 예비성형체는 종래에 제1도에 도시된 방법에 따라 주로 제조되어 왔는바, 이를 제2도에 도시된 장치를 참조하여 보다 상세히 설명하면 다음과 같다.Meanwhile, the preform has been mainly manufactured according to the method shown in FIG. 1, which will be described in more detail with reference to the apparatus shown in FIG.
먼저 덩어리 상태로 뭉쳐져 있는 단섬유, 휘스커, 입자등 세라믹 강화재를 물, 알코올등과 같은 수성 분산매질과 혼합하여 균일하게 분산시켜 강화재 수용액을 형성시킨 다음, 형성된 강화재 수용액에 바인더를 첨가 혼합하여 강화재 혼합액을 제조하고, 그 혼합액을 제2도에 도시된 장치의 상부로 주입하여 강화재 성분을 침지시키면서 하부 배출구(5)로부터 진공펌프를 이용하여 강화재 이외의 성분인 물, 알코올 및 바인더를 필터(4)를 통해 하부로 배출시키면, 상부의 침지된 강화재 응집체인 예비성형체가 남게 된다.First, the ceramic reinforcing materials, such as short fibers, whiskers, and particles, which are aggregated in the form of agglomerates, are mixed with an aqueous dispersion medium such as water and alcohol to uniformly disperse to form an aqueous reinforcing material solution. And a mixture of water, alcohol and a binder other than the reinforcing material by using a vacuum pump from the lower outlet 5 while immersing the reinforcing material component by injecting the mixed solution into the upper portion of the apparatus shown in FIG. When discharged through the bottom, the preform, which is the aggregate of the upper immersion reinforcement remains.
이같은 응집상태의 예비성형체를 회수하여 원하는 부피로 제어한 후 오븐등에 의해 가열하여 건조시켜 원하는 예비성형체를 제조하였다.The preform in the form of agglomerated state was recovered and controlled to a desired volume, and then heated and dried in an oven to prepare a desired preform.
상기와 같은 종래의 예비성형체 제조방법에 있어서는 예비성형체가 일정한 강도를 갖도록 무기질 바인더를 첨가하여야 하나, 이같이 첨가되는 무기질 바인더의 량에 따라 예비성형체의 물성도 달라지게 되어 최적물성을 얻기 위한 바인더의 량을 별도로 결정하여야 하는 등 번거로운 문제점이 있는 것이다.In the conventional method of manufacturing a preform as described above, an inorganic binder should be added so that the preform has a certain strength, but the physical properties of the preform also vary according to the amount of the inorganic binder added as described above. There are troublesome problems such as having to decide separately.
이에 본 발명의 목적은 종래에 사용되던 수성분산매질 및 무기질 바인더를 사용하지 않는 보다 개선된 예비성형체 제조방법을 제공하는데 있다.Accordingly, an object of the present invention is to provide an improved method for preparing a preform, which does not use an aqueous acid medium and an inorganic binder, which are conventionally used.
본 발명의 다른 목적은 무기질 바인더를 사용하지 않고도 일정강도를 유지할 수 있는 보다 개선된 예비성형체 제조방법을 제공하는데 있다.Another object of the present invention is to provide an improved method for producing a preform that can maintain a certain strength without using an inorganic binder.
본 발명에 의하면, 시리콘 오일 1리터(L)당 세라믹 강화재 0.5-2중량% 비율로 실리콘 오일과 세라믹 강화재를 혼합한 후 교반하여 세라믹 강화재의 실리콘 오일 분산물을 제조하고, 그 결과물인 실리콘 오일 분산물로부터 실질적인 량의 실리콘 오일을 여과하여 제거하여 강화재응집체를 형성하고, 강화재 응집체를 원하는 부피분률로 조절하고 나서 건조시켜 함유된 실리콘 오일을 제거하여 건조 예비성형체를 제조하고, 상기 건조 예비성형체를 내부 함유된 잔류 실리콘 오일이 대기중의 산소와 반응하여 SiO2를 형성하도록 대기중에서 열처리함, 을 포함하는 금속복합 재료 제조용 예비성형체 제조방법이 제공된다.According to the present invention, a silicone oil dispersion of a ceramic reinforcing material is prepared by mixing and stirring the silicone oil and the ceramic reinforcing material at a ratio of 0.5-2% by weight of the ceramic reinforcing material per liter of silicone oil (L), and the resulting silicone oil A substantial amount of silicone oil is filtered off from the dispersion to form reinforcement aggregates, the reinforcement aggregates are adjusted to the desired volume fraction and dried to remove the contained silicone oil to prepare a dry preform, and the dry preform is A method for producing a preform for producing a metal composite material is provided, wherein the residual silicone oil contained therein is heat treated in the atmosphere to react with oxygen in the atmosphere to form SiO 2 .
이하, 본 발명에 대하여 상세히 설명한다.EMBODIMENT OF THE INVENTION Hereinafter, this invention is demonstrated in detail.
본 발명에서는 종래의 예비성형체 제조시 사용되던 물, 알코올 등 수성 분산매질 및 결합제로 사용하던 무기질 바인더를 사용하지 않고, 대신 실리콘 오일을 세라믹 강화재용 분산매질로 사용함으로써 세라믹 강화재를 분산시킨 다음 건조 및 열처리를 거침으로써 실리콘 오일의 산화에 따른 SiO2형성으로 인해 세라믹 강화재가 서로 결합이 되고 나아가 결과 산물인 예비성형체가 일정강도를 갖게 하는 것이다.In the present invention, the inorganic reinforcing media such as water and alcohol, which are used in the preparation of the preform, and the inorganic binder used as the binder, are used instead of the silicone reinforcing material by dispersing the ceramic reinforcing material and then drying and By heat treatment, the ceramic reinforcing materials are bonded to each other due to the formation of SiO 2 due to the oxidation of the silicone oil, and the resultant preform has a certain strength.
본 발명의 방벙에 사용되는 세라믹 강화재로서는 단섬유, 휘스커, 입자등 통상의 세라믹 강화재를 사용할 수 있다.As the ceramic reinforcing material used in the method of the present invention, ordinary ceramic reinforcing materials such as short fibers, whiskers and particles can be used.
또한, 본 발명의 방법에 사용될 수 있는 실리콘 오일은 강호재의 밀도(3.3)를 고려하여 1-5cs 정도의 낮은 점도의 것이 좋다.In addition, the silicone oil that can be used in the method of the present invention is preferably of a low viscosity of about 1-5cs in consideration of the density of the strong material (3.3).
실리콘 오일의 점도가 크게 되면 교반후 예비성형체 제조장치에 주입할 경우 세라믹 강화재의 침전속도가 느리게 되기 때문이다.If the viscosity of the silicone oil is large, the precipitation rate of the ceramic reinforcing material is slow when injected into the preform manufacturing apparatus after stirring.
한편, 분산매질인 실리콘 오일에 혼합되는 세라믹 강화재의 량은 실리콘 오일1리터(L)당 세라믹 강화재를 중량비로 0.5-2% 혼합 분산시키는 것이 바람직하다.On the other hand, the amount of ceramic reinforcing material to be mixed in the silicone oil of the dispersion medium is preferably mixed and dispersed 0.5-2% by weight ratio of the ceramic reinforcing material per 1 liter (L) of silicone oil.
세라믹 강화재의 량이 2%를 넘게 되면 일방향 배향시 실리콘 오일내에 세라믹 강화재의 밀도가 높게 되어 일방향 배향시 서로 엉키는 현상이 발생되어 배향이 곤란하게 되며, 반면 0.5% 이하로 되면 예비성형체 제조시 강화재의 일방향 배향은 가능하지만 원하는 부피의 예비성형체 제조시 시간이 많이 소요되는 문제점이 있는 것이다.When the amount of ceramic reinforcing material exceeds 2%, the density of ceramic reinforcing material becomes high in the silicone oil in one-way orientation, and entanglement occurs in one-way orientation, which makes it difficult to align. Orientation is possible, but there is a problem that takes a long time when preparing the preform of the desired volume.
본 발명의 방법에서 세라믹 강화재를 실리콘 오일에 혼합하여 균일하게 분산시키기 위하여 기계적 교반기, 마그네틱 교반기등과 같은 교반기 뿐만 아니라 초음파를 이용할 수도 있다.In the method of the present invention, an ultrasonic wave may be used as well as a stirrer such as a mechanical stirrer, a magnetic stirrer, etc. to uniformly disperse the ceramic reinforcing material in the silicone oil.
이와 같이 실리콘 오일에 세라믹 강화재를 분산시켜 형성한 세라믹 강화재의 실리콘 오일 분산물은 흡인여과하여 실리콘 오일을 흡인하게 되며, 흡인후 여과되지 않은 실리콘 오일-함유 세라믹 강화재(강화재 응집체)는 장치로부터 회수한 후 원하는 부피 분율을 갖도록 조절하여 예비성형체를 형성한다.Thus, the silicone oil dispersion of the ceramic reinforcing material formed by dispersing the ceramic reinforcing material in the silicone oil is suction filtered to suck the silicon oil, and the unfiltered silicon oil-containing ceramic reinforcing material (reinforcement aggregate) is recovered from the device after suction. It is then adjusted to have the desired volume fraction to form a preform.
그후 함유된 실리콘 오일이 거의 전부(약 98%정도) 제거되도록 질소분위기하에서 가열 건조시키게 된다. 건조는 150-180℃에서 2-4시간 정도 건조시키는 것이 바람직하다.The silicon oil is then dried under nitrogen atmosphere to remove almost all of the silicone oil (approximately 98%). It is preferable to dry at 150-180 degreeC for 2-4 hours.
건조된 예비성형체는 열처리 과정을 거치게 되면 열처리 과정에서 예비성형체 내부에 잔류하는 실리콘 오일중의 실리콘이 공기중의 산소와 반응하여 SiO2를 형성하게 되고, 이는 예비성형체를 구성하는 세라믹 강화재의 접촉부분에 생성되어 강화재까지 결합을 하게 되고 그 결과 예비성형체로 하여금 필요한 강도를 갖게 하는 것이다.When the dried preform undergoes a heat treatment process, silicon in the silicone oil remaining inside the preform reacts with oxygen in the air to form SiO 2 in the heat treatment process, which is formed on the contact portion of the ceramic reinforcing material constituting the preform. It creates and bonds to the reinforcement, which gives the preform the strength it needs.
열처리는 실리콘 오일의 Si 이 산소와 반응할 수 있는 조건이면 좋으며, 바람직하게는 800-850℃에서 20분-40분 정도 유지하는 것이 좋다.The heat treatment may be a condition in which Si of the silicone oil can react with oxygen, and preferably, 20 to 40 minutes is maintained at 800-850 ° C.
상기한 바와 같이 본 발명의 방법에 의하면 예비성형체 제조시 무기질 바인더를 첨가하지 않고도 SiO2형성에 의한 강도 유지가 가능할 뿐 아니라 수용성 분산매질을 사용하지 않아 그 제조공정도 단순화시킬 수 있는 것이다.As described above, according to the method of the present invention, it is possible not only to maintain the strength by forming SiO 2 without adding an inorganic binder when preparing the preform, but also to simplify the manufacturing process without using an aqueous dispersion medium.
한편, 본 발명에서 적용하고자 하는 세라믹 강화재로 된 예비성형체는 금속복합재료를 제조하는데 필요한 중간소재로서 사용되는 금속으로는 알미늄과 마그네슘등 융점이 700℃ 이하인 소재에 사용되며 알루미나 단섬유/알미늄합금, 마그네슘 합금 및 실리콘 카바이트 입자/알미늄 합금, 마그네슘 합금을 포함한다.On the other hand, the preform of the ceramic reinforcing material to be applied in the present invention is used as the intermediate material required to manufacture a metal composite material is used in a material having a melting point of 700 ℃ or less, such as aluminum and magnesium, and alumina short fiber / aluminum alloy, Magnesium alloys and silicon carbide particle / aluminum alloys, magnesium alloys.
이하, 본 발명의 실시예를 설명한다.Hereinafter, embodiments of the present invention will be described.
[실시예 1]Example 1
실리콘 오일 11에 직경 3㎛×평균길이 203㎛의 알루미나 단섬유 15gr을 넣고 마그네틱 교반기로 30분간 교반하여 알루미나 단섬유 덩어리를 균일하게 실리콘 오일에 분산시켰다.15 gr of alumina short fibers of 3 micrometers in diameter x average length of 203 micrometers were put into the silicone oil 11, and it stirred for 30 minutes with the magnetic stirrer, and the alumina short-fiber mass was disperse | distributed uniformly in silicone oil.
이같이 제조된 실리콘 오일 분산물(2)(알루미나 단섬유+실리콘 오일)을 제2도의 예비성형체 제조장치인 아크릴 본체(1)내에 주입한 후, 진공펌프를 배출구(5)에 연결하여 필터(4)를 통해 나오는 실리콘 오일을 흡인하였다.The silicone oil dispersion 2 thus prepared (alumina short fiber + silicone oil) is injected into the acrylic body 1, which is a preform manufacturing apparatus of FIG. 2, and then a vacuum pump is connected to the outlet 5 to filter 4 The silicone oil coming out through the a) was aspirated.
흡인후 여과지 위에 남은 오일-제거된 세라믹 강화재(3)을 장치로부터 꺼내어 원하는 부피분율을 갖도록 높이 조절을 하였다.After suction, the oil-removed ceramic reinforcement 3 remaining on the filter paper was taken out of the apparatus and height-adjusted to have a desired volume fraction.
이어서 상기 부피분율 제어된 오일-제거 세라믹 강화재(3)을 170℃온도로 유지된 오븐에 넣고 질소 분위기하에서 3시간 건조시켜 세라믹 강화재(3)내의 실리콘 오일함량이 약 2%정도 되게 하였다.The volume fraction controlled oil-removing ceramic reinforcement 3 was then placed in an oven maintained at 170 ° C. and dried under nitrogen atmosphere for 3 hours so that the silicone oil content in the ceramic reinforcement 3 was about 2%.
이를 다시 800℃로 승온시켜 30분간 유지한 후 냉각시켜 예비성형체를 제조하였다.This was again heated to 800 ° C. for 30 minutes and then cooled to prepare a preform.
제조된 예비성형체를 주사전자 현미경으로 관찰하였으며, 그 결과를 제4도(a)에 나타내었다.The prepared preform was observed under a scanning electron microscope, and the result is shown in FIG.
제4도(a)에 의하면 강화재인 알루미나 단섬유의 표면과 섬유와 섬유가 맞닿는 부분에 실리콘 오일중의 실리콘이 열처리시 공기중의 산소와 반응하여 SiO2가 형성된 것을 알 수 있다.According to FIG. 4 (a), it can be seen that silicon in the silicone oil reacts with oxygen in the air during heat treatment to the surface of the alumina short fibers as the reinforcing material and the fiber and the fiber contact to form SiO 2 .
반면 종래방법에 따라 제조한 예비성형체의 주사전자 현미경 관찰 결과를 보여주는 제4도(b)에 의하면 세라믹 강화제의 표면보다는 섬유와 섬유가 맞닿는 부분에 무기질 바인더가 존재함을 볼 수 있다.On the other hand, according to FIG. 4 (b) showing the scanning electron microscope observation result of the preform manufactured according to the conventional method, it can be seen that the inorganic binder exists at the portion where the fiber and the fiber abut rather than the surface of the ceramic reinforcing agent.
[실시예 2]Example 2
강호재로써 SiC 휘스커(직경 1㎛, 평균길이 10㎛)를 사용한 것을 제외하고는 실리예 1과 같은 방법으로 예비성형체를 제조하였다.A preform was prepared in the same manner as in Example 1 except that SiC whiskers (diameter 1 μm, average length 10 μm) were used as the strong material.
제조된 예비성형체에 대하여 주사전자 현미경 관찰결과 실시예 1에서와 같이 강화재의 표면과 휘스커와 휘스커가 맞닿는 부분에 SiO2가 형성되었음을 확인할수 있었다.Scanning electron microscopic observation of the prepared preform confirmed that SiO 2 was formed on the surface of the reinforcing material and the portion where the whisker and the whisker abut as in Example 1.
상기한 바와 같이 본 발명의 방법에 의하면, 분산매질로 실리콘 오일을 사용하고 그후 실리콘 오일을 열처리함으로써 실리콘 오일중의 실리콘이 공기중의 산소와 반응하여 SiO2를 형성하기 때문에 종래와 같이 무기질 바인더를 사용하지 않고 열처리에 의한 결합력을 생성하게 함으로써 공정이 단순화됨과 동시에 금속복합재료의 제조단가는 물론 예비성형체의 생산성도 향상될 수 있는 것이다 .As described above, according to the method of the present invention, since the silicon oil in the silicone oil reacts with oxygen in the air to form SiO 2 by using the silicone oil as a dispersion medium and then heat treating the silicone oil, an inorganic binder is used as in the prior art. By generating the bonding force by heat treatment instead of simplifying the process, the production cost of the metal composite material as well as the productivity of the preform can be improved.
Claims (4)
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