KR0143615B1 - A method for manufacturing c/c composites of high thermal conductivity - Google Patents

A method for manufacturing c/c composites of high thermal conductivity

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KR0143615B1
KR0143615B1 KR1019950069252A KR19950069252A KR0143615B1 KR 0143615 B1 KR0143615 B1 KR 0143615B1 KR 1019950069252 A KR1019950069252 A KR 1019950069252A KR 19950069252 A KR19950069252 A KR 19950069252A KR 0143615 B1 KR0143615 B1 KR 0143615B1
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carbon
pitch
carbon fiber
graphite
molded body
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KR970042376A (en
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이홍범
박홍식
박현철
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석진철
대우중공업주식회사
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Abstract

본 발명은 고열전도도 탄소/탄소 복합재료(C/C composites)의 제조방법에 관한 것으로, 탄소섬유와 핏치를 혼합하여 성형체를 만들고 이 성형체에 핏치를 함침,탄화시켜 탄소/탄소 복합재료를 제조하는 방법에 있어서, 상기 탄소섬유 및 핏치에 흑연을 추가적으로 흔합하여 성형체를 만들어 주되, 각 성분의 구성비를 탄소섬유 20 - 50중량%, 핏치 25 - 50중량%, 흑연 10 - 40중량%의 범위에서 선택해 줌으로써, 저렴한 비용으로 우수한 고열전도도의 탄소/탄소 복합재료를 제공해 주는 것이다.The present invention relates to a method for producing a high thermal conductivity carbon / carbon composites (C / C composites), to produce a molded body by mixing the carbon fiber and the pitch and impregnated and carbonized the molded body to produce a carbon / carbon composite material In the method, the carbon fiber and the pitch is further mixed with graphite to form a molded body, wherein the composition ratio of each component is selected in the range of 20-50 wt% carbon fiber, 25-50 wt% pitch, and 10-40 wt% graphite. This provides a high thermal conductivity carbon / carbon composite at low cost.

Description

고열전도도 탄소/탄소 복합재료의 제조방법.Method for producing high thermal conductivity carbon / carbon composites.

제1도는 본 발명의 제1실시예에 따른 제조방법의 공정도,1 is a process chart of the manufacturing method according to the first embodiment of the present invention,

제2도는 본 발명의 재2실시애에 따른 제조방법의 공정도,2 is a process chart of the manufacturing method according to the second embodiment of the present invention,

제3도는 종래 제조방법의 일예에 따른 공정도이다.3 is a process chart according to an example of the conventional manufacturing method.

본 발명은 탄소/탄소 복합재료(C/C composites)의 제조방법에 관한 것으로, 특히 핏치를 탄소기지물질로 하는 탄소/탄소 복합재료의 고열전도도 특성을 향상시켜 주는 탄소/탄소 복합재료의 제조방법에 관한 것이다.The present invention relates to a method for manufacturing carbon / carbon composites, and in particular, a method for producing a carbon / carbon composite material that improves high thermal conductivity characteristics of a carbon / carbon composite material having pitch as a carbon base material. It is about.

일반적으로 탄소/탄소 복합재료는 가벼우면서도 강도가 뛰어나고 고온 및 내열특성 등이 우수하여 내열재료로 각광을 받고 있는 소재인데, 이와 같이 탄소/탄소 복합재료는 고온분위기에 노출된 상태로 많이 사용되어지기 때문에 고온상태에서 더욱 우수한 열전도성과 열안정성을 가질 필요가 있다. 특히, 많은 에너지를 흡수해야 하는 경우 흡수된 에너지가 대부분 열로 전환되어 접촉면의 온도가 2,500℃ 이상의 고온으로 급격히 상승하게 되는 경우가 많은데, 이 경우 빠른 열방출을 위해 열접측면의 두께와 원주방향에 대해 높은 열전도도 특성이 요구된다.In general, carbon / carbon composites are light and excellent in strength and excellent in high temperature and heat resistance. Therefore, carbon / carbon composites are widely used in high temperature atmospheres. Therefore, it is necessary to have better thermal conductivity and thermal stability at high temperature. In particular, when a large amount of energy needs to be absorbed, the absorbed energy is converted into heat, and thus the temperature of the contact surface is rapidly increased to a high temperature of more than 2,500 ° C. High thermal conductivity properties are required.

한편, 탄소/탄소 복합재료(C/C composites)는 탄소섬유 강화재와 탄소기지물질로 구성되는 것으로, 탄소섬유 강화재료는 폴리아크릴로니트릴(polyacrylonitrile, PAN)계 , 핏치계 등이 있고, 탄소기지로는 페놀수지, 퓨란수지, 핏치, 열분해탄소(CVD) 등이 있는데, 탄소/탄소 복합재료의 열전도도 특성은 이와 같은 구성 원료의 종류에 따라 많은 영향을 받을 뿐만 아니라, 탄소섬유와 탄소기지의 열처리 온도, 탄소섬유의 배향성 등의 여러 가지 요인에 영향을 받는다.Meanwhile, C / C composites are composed of carbon fiber reinforcement and carbon base materials, and carbon fiber reinforcement materials include polyacrylonitrile (PAN) and pitch systems. Examples include phenol resins, furan resins, pitches, and pyrolytic carbon (CVD). The thermal conductivity of carbon / carbon composites is not only influenced by the type of constituent raw materials, but also by carbon fiber and carbon base. It is influenced by various factors such as the heat treatment temperature and the orientation of the carbon fibers.

따라서 탄소/탄소 복합재료의 재조시 열전도도 특성에 영향을 미치는 여러가지 변수를 잘 조합하여 최적의 열전도도 특성을 갖도록 해 주는 것이 중요한데, 이는 여간 쉬운일이 아니다.Therefore, it is important to combine the various parameters affecting the thermal conductivity properties of the carbon / carbon composite material in order to have the optimum thermal conductivity properties, which is not easy.

종래에 탄소/탄소 복합재료의 열전도도를 향상시키기 위해 강화재로 고열전도도 핏치계 탄소섬유를 사용한 것이 있으나, 이는 가격이 매우 비싼 문제가 있으며, 또한 고온에서 흑연화 처리를 하여 탄소/탄소 복합재료를 제조함으로써 열전도도를 향상시켜 주는 방법이 일반적으로 많이 이용되었는데, 이는 에너지가 많이 소모되어 원가가 높고 기계적 강도에도 나쁜 영향을 미치는 문제점이 있었다.Conventionally, high thermal conductivity pitch-based carbon fiber is used as a reinforcing material to improve the thermal conductivity of the carbon / carbon composite material. However, this is a very expensive problem, and the carbon / carbon composite material is subjected to graphitization at a high temperature. By manufacturing, a method of improving thermal conductivity has been generally used, which has a problem of high energy consumption and high cost, and adversely affect mechanical strength.

이에 본 발명은 상기한 바와같은 종래의 문재점을 해결하기 위하여, 저렴한 비용으로 고열전도도 특성을 크게 향상시켜 줄 수 있는 탄소/탄소 복합재료(C/C composites)의 제조방법을 제공하는데 그 목적이 있다.Accordingly, an object of the present invention is to provide a method of manufacturing carbon composite materials (C / C composites) that can significantly improve high thermal conductivity characteristics at low cost in order to solve the conventional problems as described above. .

상기한 바와 같은 목적을 달성하기 위한 본 발명에 탄소/탄소 복합재료의 제조방법은, 탄소섬유와 핏치를 혼합하여 성형체를 만들고 이 성형체에 핏치를 함침,탄화시켜 탄소/탄소 복합재료를 제조하는 방법에 있어서, 상기 탄소섬유 및 핏치에 흑연을 추가적으로 혼합하여 성형체를 만들어 주는 것을 특징으로 한다.Method for producing a carbon / carbon composite material in the present invention for achieving the above object, a method of manufacturing a carbon / carbon composite material by mixing the carbon fiber and the pitch to form a molded body, impregnated and carbonized the molded body In the, characterized in that to form a molded body by further mixing the graphite with the carbon fiber and pitch.

이하 본 발명을 첨부된 예시도면을 참조하여 상세히 설명한다.Hereinafter, the present invention will be described in detail with reference to the accompanying drawings.

본 발명의 탄소/탄소 복합재료 재조방법에서 종래의 방법과 상이한 특징점은, 탄소섬유 및 핏치에 흑연을 추가적으로 첨가하여 성형체를 만들어 주는 점에 있다.In the carbon / carbon composite material manufacturing method of the present invention, a different feature point from the conventional method is that the graphite is added to the carbon fiber and the pitch to form a molded body.

이때 각 성분의 구성비는 탄소섬유 20 - 50중량%, 핏치 25중량%, 흑연 10 - 40중량%의 범위에서 선택하여 준다.At this time, the composition ratio of each component is selected from the range of 20-50% by weight of carbon fiber, 25% by weight of pitch, 10-40% by weight of graphite.

그리고 본 발명에서 흑연을 첨가하여 성형체를 제조하는 방법은 두가지 형태가 있는데, 첫째 방법은, 탄소섬유를 절단한 상태로 핏치 및 흑연과 흔합하여 슬러리 상태로 만들고 프레스에서 성형해 준는 방법이다.In the present invention, there are two forms of a method of manufacturing a molded body by adding graphite, and the first method is a method of forming a slurry by mixing with pitch and graphite in a state of cutting carbon fibers and molding in a press.

이때, 탄소섬유는 골고루 혼합이 잘되도록 200㎛ 내지 2mm정도의 크기로 절단하여 주면 좋고, 핏치와 흑연의 입도는 0.5㎛ 내지 10㎛ 정도로 분쇄한 것을 사용하면 바람직하다. 만약, 각 조성물이 균일하게 잘 혼합이 되지 않으면, 미세조직의 불균일 및 기공의 형성 등으로 인하여 강도의 저하, 열전도도의 불량 등의 문제점이 생길 수 있으므로, 각 구성물의 입도 흑은 크기와 첨가량을 적절히 맞추어 주는 것은 대단히 중요하다.In this case, the carbon fiber may be cut to a size of about 200 μm to 2 mm so as to be evenly mixed, and the particle size of the pitch and graphite is preferably about 0.5 μm to 10 μm. If each composition is not well mixed uniformly, problems such as a decrease in strength and poor thermal conductivity may occur due to the nonuniformity of the microstructure and the formation of pores. It's very important to get it right.

둘째 방법은, 핏치와 흑연을 균일하게 혼합하고, 이 혼합물을 직물형태의 탄소섬유에 골고루 뿌린 후 가열하여 프리프레그를 만들어서 이 프리프레그를 적층하여 성형해 주는 방법이다.In the second method, the pitch and graphite are uniformly mixed, and the mixture is evenly sprayed on the carbon fiber in the form of fabric and then heated to form a prepreg, which is then laminated and molded.

여기에서 핏치와 흑연의 입도는 상기와 등일하게 해주고, 가열온도는 180 - 27O℃의 범위로 하여 준다.Here, the pitch and the particle size of the graphite is equal to the above, and the heating temperature is in the range of 180-2 O70.

한편, 상기 첫째와 둘째 방법을 혼합한 방법으로서, 둘째방법으로 만든 프리프레그와 첫째방법에서의 절단섬유, 핏치 및 흑연 혼합물을 교대로 적층하여 성형해 주는 방법을 사용할 수도 있다.On the other hand, as a method of mixing the first and second methods, it is also possible to use a method of alternately laminating the prepreg made in the second method and the chopped fiber, pitch and graphite mixture in the first method.

그리고 상기에서 탄소섬유는 PAN계 탄소섬유로 사용하는 것이 바람직하고, 또 열전도도를 더욱 향상시켜 주기 위해 탄소섬유를 아르곤 분위기 하에서 2,000 - 3,OOO℃의 온도로 고온 열처리하여 혹연화 처리를 하여 주면 더욱 바람직하다.In the above, the carbon fiber is preferably used as a PAN-based carbon fiber, and in order to further improve thermal conductivity, the carbon fiber is subjected to a high temperature heat treatment at a temperature of 2,000-3, OOO ° C. under an argon atmosphere to be subjected to a quenching treatment. More preferred.

이상에서 설명한 바와 같은 방법으로 제조한 성형체는, 탄화 및 흑연화 처리를 한 후, 다시 핏치를 함침하여 탄화 및 흑연화 처리를 반복하는 밀도화 공정을 소정의 밀도가 얻어질 때까지 수행하여 주면 고열전도도 탄소/탄소 복합재료가 제조되게 되는 것이다.The molded article produced by the method described above is subjected to a carbonization and graphitization treatment, and then subjected to a densification step of impregnating a pitch to repeat the carbonization and graphitization treatment until a predetermined density is obtained. Conductivity carbon / carbon composites will be produced.

한편, 본 발명의 구체적인 여러 실시예에 따라 탄소/탄소 복합재료를 제조하여 그 열전도도를 테스트하여 보았는 바, 이하에서는 이를 설명 한다.Meanwhile, according to various embodiments of the present invention, the carbon / carbon composite material was manufactured and tested for thermal conductivity thereof. Hereinafter, this will be described.

[실시예1]Example 1

제1도에 실시예 1의 재조공정도가 도시되어 있는 바와 같이, 핏치와 흑연을 분쇄기에서 0.5 - lO㎛의 입도 크기로 미리 분쇄하여 균일하게 혼합하고, 이 혼합물을 PAN계 탄소섬유 직물위에 골고루 뿌려서 180 - 27O℃의 온도범위로 가열하여 프리프레그를 제조하였다. 이 프리프레그를 적층하여 성형체를 만들어서 탄화 및 흑연화처리를 한 후, 다시 핏치를 함침,탄화시켜 탄소/탄소 복합재료를 제조하였다.As shown in FIG. 1, the manufacturing process chart of Example 1 is preliminarily pulverized in a pulverizer to a particle size of 0.5-10 탆 in a pulverizer and uniformly mixed, and the mixture is evenly sprayed onto the PAN-based carbon fiber fabric. Prepregs were prepared by heating to a temperature range of 180-2 O < 0 > C. The prepreg was laminated to form a molded body, carbonized and graphitized, and then impregnated and carbonized to produce a carbon / carbon composite material.

[실시예2]Example 2

제2도에 실시예 2의 재조공정도가 도시 되어 있는 바와 같이, PAN계 탄소섬유를 아르곤 분위기하에서 2,000 - 3,OOO℃의 온도로 고온 열처리를 한 후 섬유절단기에서 200㎛ - 2mm길이로 절단하여 혼합통에서 핏치와 인조흑연을 골고루 흔합한다. 이때 핏치와 흑연은 실시예1 과 같이 미리 분쇄기에서 0.5 - l0㎛의 입도크기로 분쇄한 것을 사용한다. 이 흔합물을 프래스에 의해 성형체를 제조하여 탄화 및 흑연화 처리를 한 후, 다시 핏치를 함침, 탄화시켜 탄소/탄소 복합재료를 제조하였다.As shown in FIG. 2, the manufacturing process chart of Example 2 was subjected to a high temperature heat treatment of PAN-based carbon fiber at a temperature of 2,000-3, OOO ° C. under argon atmosphere, and then cut to 200 μm-2 mm length in a fiber cutter. Evenly mix the pitch and artificial graphite in the mixing bowl. At this time, the pitch and graphite is used in the crusher in the same mill as the particle size of 0.5-10㎛ previously. This mixture was produced by molding a carbonized product, subjected to carbonization and graphitization treatment, and then impregnated and carbonized to produce a carbon / carbon composite material.

[실시예3]Example 3

실시예1에서 만든 프리프레그의 양면에 실시예 2에서 만든 혼합물층을 대고 프리폼을 만들어서, 프레스에 의해 성형체를 제조하여 탄화 및 혹연화 처리를 한 후, 다시 핏치를 함침, 탄화시켜 탄소/탄소 복합 재료를 제조 하였다.Preforms are prepared by placing the mixture layer prepared in Example 2 on both sides of the prepreg prepared in Example 1, and a molded body is manufactured by pressing, followed by carbonization and derivatization treatment, and then impregnated and carbonized to form a carbon / carbon composite. The material was prepared.

[비교예][Comparative Example]

제3도에 도시된 바와 같은 종래의 방법으로 탄소섬유와 핏치를 이용하여 프리프레그를 만들고, 이를 적층,성형하여 탄화 및 흑연화시킨 다음, 다시 핏치를 함침,탄화시키고, 상기 실시예와는 달리 흑연화 처리를 추가 실시하여 탄소/탄소 복합재료를 제조하였다. 상기의 실시애 1,2,3 및 비교예에 따라 제조한 탄소/탄소 복합재료에 대해 열전도도를 측정 비교하여 본 결과는 다음의 도표와 같았다.Prepreg using carbon fiber and pitch as shown in FIG. 3 is made, carbonized and graphitized by laminating and molding it, and then impregnating and carbonizing the pitch, unlike the above embodiment. Graphitization treatment was further performed to produce carbon / carbon composites. The thermal conductivity of the carbon / carbon composite materials prepared according to Examples 1, 2, and 3 and Comparative Examples was measured and compared.

*실시예 1,2,3의 열 전도도값은 비교예의 열 도도를 기준으로 하여 산정한 것임.* The thermal conductivity values of Examples 1,2 and 3 are calculated based on the thermal conductivity of the comparative example.

상기의 도표에서 보는 바와 같이 본 발명의 재조방법에 따라 제조한 탄소/탄소 복합재료는 종래의 것에 비해 열전도도가 휠씬 뛰어남을 알 수 있으며, 또한 상대적으로 저렴한 PAN계 탄소섬유를 사응하거나 또는 고온에서의 흑연화 처리 횟수를 종래에 비해 줄여 주어도, 열전도도가 우수한 탄소/탄소 복합재료를 제조할 수 있으므로, 본 발명의 제조방법은 제조원가를 절감시켜 주고, 흑연화 처리에 따른 기계적 강도의 저하염려를 방지해 줄 수 있게 된다.As shown in the above diagram, it can be seen that the carbon / carbon composite material prepared according to the manufacturing method of the present invention has a much higher thermal conductivity than the conventional one, and also corresponds to a relatively inexpensive PAN-based carbon fiber or at a high temperature. Even if the number of graphitization treatments is reduced compared to the prior art, since the carbon / carbon composite material having excellent thermal conductivity can be manufactured, the manufacturing method of the present invention can reduce the manufacturing cost and reduce the mechanical strength caused by the graphitization treatment. You can prevent it.

Claims (10)

탄소섬유와 핏치를 혼합하여 성형체를 만들고 이 성형체에 핏치를 함침,탄화시켜 탄소/탄소 복합재료를 제조하는 방법에 있어서, 상기 탄소섬유 및 핏치에 흑연을 추가적으로 혼합하여 성형체를 만들어 주는 것을 특징으로 하는 탄소/탄소 복합재료의 재조방법.A method of manufacturing a carbon / carbon composite material by mixing a carbon fiber and a pitch to form a molded body, and impregnating and carbonizing the molded body, wherein the carbon fiber and the pitch are further mixed with graphite to form a molded body. How to make carbon / carbon composites. 제1항에 있어서, 상기 탄소섬유는 20 - 50중량%, 핏치는 25 - 50중량%, 흑연은 10 - 40중량%의 조성비 범위로 흔합해 주는 것을 특징으로 하는 탄소/탄소 복합재료의 제조방법.According to claim 1, wherein the carbon fiber is 20 to 50% by weight, pitch is 25 to 50% by weight, graphite is 10 to 40% by weight of the composition of the carbon / carbon composite material manufacturing method characterized in that it is mixed . 제1항에 있어서, 상기 핏치와 흑연은 그 입도를 0.5㎛ 내지 10㎛범위로 분쇄한 것을 사용하는 것을 특징으로 하는 탄소/탄소 복합 재료의 제조방법.The method of claim 1, wherein the pitch and the graphite are pulverized in a particle size of 0.5 μm to 10 μm. 제1항에 있어서, 상기 탄소섬유는 PAN계 탄소섬유인 것을 특징으로 하는 탄소/탄소 복합재료의 재조방법.The method of claim 1, wherein the carbon fiber is a PAN-based carbon fiber. 제1항에 있어서, 상기 탄소섬유는 아르곤 분위기하에서 2,000 - 3,OOO℃의 온도로 고온 열처리하여 사용하는 것을 특징으로 하는 탄소/탄소 복합재료의 제조방법.The method of claim 1, wherein the carbon fiber is heat-treated at a temperature of 2,000-3, OOO ° C. under an argon atmosphere. 제1항에 있어서, 상기 탄소섬유를 절단한 상태로 핏치 및 흑연과 혼합하여 슬러리 상태로 만들고 프레스에서 성형하여 성형체를 만들어 주는 것을 특징으로 하는 탄소/탄소 복합재료의 제조방법.The method of claim 1, wherein the carbon fiber is cut and mixed with pitch and graphite to form a slurry and molded in a press to form a molded body. 제6항에 있어서, 상기 탄소섬유를 200㎛ 내지 2mm의 크기로 절단해 주는 것을 특징으로 하는 탄소/탄소 복합재료의 제조방법.The method of claim 6, wherein the carbon fiber is cut into a size of 200 μm to 2 mm. 제1항에 있어서, 상기 핏치와 흑연을 균일하게 혼합하고, 이 혼합물을 직물형태의 탄소섬유에 골고루 뿌린 후 가열하여 프리프레그를 만들어서 이 프리프레그를 적층하여 성형체를 만들어 주는 것을 특징으로 하는 탄소/탄소 복합재료의 제조방법.The method according to claim 1, wherein the pitch and graphite are uniformly mixed, and the mixture is evenly sprinkled on the carbon fiber in the form of fabric and then heated to make a prepreg, and the prepreg is laminated to form a molded body. Method for producing a carbon composite material. 제8항에 있어서, 상기 가열온도를 180 - 27O℃로 해주는 것을 특징으로 하는 탄소/탄소 복합재료의 제조방법．9. The method for producing a carbon / carbon composite material according to claim 8, wherein the heating temperature is 180-2O < 0 > 제8항에 있어서, 상기 프리프레그를 적층하는 사이에 절단한 탄소섬유, 핏치 및 흑연의 흔합물을 추가로 적층해 주는 것을 특징으로 하는 탄소/탄소 북합재료의 제조방법.The method of producing a carbon / carbon composite material according to claim 8, further comprising laminating a mixture of carbon fiber, pitch and graphite cut between the prepregs.
KR1019950069252A 1995-12-30 1995-12-30 A method for manufacturing c/c composites of high thermal conductivity KR0143615B1 (en)

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