KR100217435B1 - Self lubricating polyphenylene sulfide composite materials and their preparation process - Google Patents

Self lubricating polyphenylene sulfide composite materials and their preparation process Download PDF

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KR100217435B1
KR100217435B1 KR1019950039720A KR19950039720A KR100217435B1 KR 100217435 B1 KR100217435 B1 KR 100217435B1 KR 1019950039720 A KR1019950039720 A KR 1019950039720A KR 19950039720 A KR19950039720 A KR 19950039720A KR 100217435 B1 KR100217435 B1 KR 100217435B1
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polyphenylene sulfide
weight
composite material
carbon fiber
graphite powder
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KR1019950039720A
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Korean (ko)
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KR970027216A (en
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김진태
민병일
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이구택
포항종합제철주식회사
신현준
재단법인포항산업과학연구원
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L81/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing sulfur with or without nitrogen, oxygen or carbon only; Compositions of polysulfones; Compositions of derivatives of such polymers
    • C08L81/02—Polythioethers; Polythioether-ethers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
    • C08J5/0405—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres
    • C08J5/041—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres with metal fibres
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K3/04—Carbon
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/02—Fibres or whiskers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/02—Fibres or whiskers
    • C08K7/04—Fibres or whiskers inorganic
    • C08K7/06—Elements

Abstract

본 발명은 50-85중량의 폴리페닐렌설파이드, 10-30중량의 탄소섬유 및 5-20중량의 흑연 분말로 구성되는 자체윤활성을 갖는 폴리페닐렌설파이드 복합재료, 및 50-85중량의 폴리페닐렌설파이드를 가열용융하고, 5-20중량의 흑연분말을 기계적으로 혼합한 후, 10-30중량의 탄소섬유를 첨가하여 기계적으로 혼합하여 성형하는 것으로, 구성되는 자체윤활성을 갖는 폴리페닐렌설파이드 복합재료의 제조방법에 관한 것이다.50-85 weight of the present invention Polyphenylene sulfide, 10-30 weight Carbon fiber and 5-20 weight Self-lubricating polyphenylene sulfide composite material composed of graphite powder, and 50-85 weight 5-20 weight of the polyphenylene sulfide by heat-melting 10-30 weight after mechanically mixing graphite powder It is related with the manufacturing method of the polyphenylene sulfide composite material which has the self-lubrication comprised by adding carbon fiber of this, and mechanically mixing.

Description

자체윤활성을 가진 폴리페닐렌설파이드 복합재료 및 그 제조방법Polyphenylene sulfide composite material having self-lubricating activity and its manufacturing method

제1도는 탄소섬유의 함량 변화에 따른 강도 변화를 나타낸 그래프.1 is a graph showing the change in strength according to the change in the content of carbon fiber.

제2도는 탄소섬유의 함량 변화에 따른 탄성율 변화를 나타낸 그래프.2 is a graph showing a change in elastic modulus according to the change of the carbon fiber content.

제3도는 탄소섬유의 함량 변화에 따른 마찰계수 변화를 나타낸 그래프.3 is a graph showing a change in the friction coefficient according to the change of the carbon fiber content.

제4도는 흑연분말의 함량 변화에 따른 강도 변화를 나타낸 그래프.4 is a graph showing the change in strength according to the change in the content of graphite powder.

제5도는 탄소섬유의 함량 변화에 따른 마찰계수 변화를 나타낸 그래프.5 is a graph showing a change in the friction coefficient according to the change in the content of carbon fiber.

본 발명은 자체윤활성을 가진 폴리페닐렌설파이드 복합재료 및 그 제조방법에 관한 것이며, 보다 상세하게는 폴리페닐렌설파이드 수지, 탄소섬유, 및 흑연분말로 구성된 자체윤활성을 가진 폴리페닐렌설파이드 복합재료 및 그 제조방법에 관한 것이다.The present invention relates to a polyphenylene sulfide composite material having self-lubricating activity and a method for manufacturing the same, and more particularly, to a polyphenylene sulfide composite material having self-lubricating activity composed of polyphenylene sulfide resin, carbon fiber, and graphite powder; It relates to a manufacturing method.

자동차의 클러치나 기어등에는 주로 나일론과 유리섬유로 제조된 복합재료가 주로 사용되고, 그 외에도 자동차의 부품가운데 우수한 내마모성이 요구되는 부품에는 이러한 나일론 복합재료가 주로 사용되어 왔다. 그런데, 이들 나일론 복합재료의 경우 200℃ 이상의 온도에서는 사용이 불가능하고, 마찰계수의 값이 0.3 정도로 내마모성 면에서도 개선이 필요하였다.The composite material mainly made of nylon and glass fiber is mainly used for clutches and gears of automobiles. In addition, such nylon composite materials have been mainly used for parts requiring excellent wear resistance in the parts of automobiles. However, these nylon composites cannot be used at a temperature of 200 ° C. or higher, and a friction coefficient of about 0.3 is required for improvement in wear resistance.

이러한 점을 감안하여 한국 특허출원 제93-21353호에는 폴리에테르 에테르 케톤 및 폴리아미드 아미드 복합재료가 적용되었으나, 이들 원료수지의 가격이 고가이고 350-380℃의 높은 가공온도를 가지고 있기 때문에 작업상의 어려움이 있었다. 또한 한국 특허출원 제93-12389호에는 열경화성 고분자 복합재료에 대해 개재하고 있으나, 이 경우에는 고온에서 사용이 불가능하며 재활용이 불가능하여 환경문제를 일으키고 대량생산을 위한 사출성형이 어려운 단점이 있었다.In view of this, Korean Patent Application No. 93-21353 used polyether ether ketone and polyamide amide composite materials, but since these raw resins are expensive and have a high processing temperature of 350-380 ° C, There was a difficulty. In addition, Korean Patent Application No. 93-12389 discloses a thermosetting polymer composite material, but in this case, it cannot be used at a high temperature and cannot be recycled, which causes environmental problems and injection molding for mass production is difficult.

또한 현재 일반적으로 사용되는 금속을 모재로 하는 복합재료는 화학적 분위기에서 부식되기 쉬워 그 수명에 근본적으로 한계가 있었다.In addition, the metal-based composite materials that are commonly used in the present invention are prone to corrosion in a chemical atmosphere, and their lifespan is fundamentally limited.

따라서, 본 발명의 목적은 상기의 문제점을 해결하여 내열성과 내마모성이 우수한 복합재료를 제공하는 것이다.Accordingly, it is an object of the present invention to solve the above problems and to provide a composite material having excellent heat resistance and wear resistance.

본 발명의 다른 목적은 대량생산을 위한 사출성형이 가능한 복합재료를 제공하는 것이다.Another object of the present invention is to provide a composite material capable of injection molding for mass production.

본 발명의 또다른 목적은 화학적 분위기에서 내식성이 우수한 복합재료를 제공하는 것이다.It is another object of the present invention to provide a composite material having excellent corrosion resistance in a chemical atmosphere.

본 발명의 복합재료는 50-85중량의 폴리페닐렌설파이드, 10-30중량의 탄소섬유 및 5-20중량의 흑연분말로 구성되는 것을 특징으로 한다.The composite material of the present invention is 50-85 weight Polyphenylene sulfide, 10-30 weight Carbon fiber and 5-20 weight It is characterized by consisting of graphite powder.

또한 본 발명의 복합재료의 제조방법은 50-85중량의 폴리페닐렌설파이드를 가열용융하고, 5-20중량의 흑연분말을 기계적으로 혼합한 후, 10-30중량의 탄소섬유를 첨가하여 기계적으로 혼합하여 성형하는 것으로 구성되는 것을 특징으로 한다.In addition, the method for producing a composite material of the present invention is 50-85 weight 5-20 weight of the polyphenylene sulfide by heat-melting 10-30 weight after mechanically mixing graphite powder It is characterized by consisting of the addition of the carbon fiber of the mechanical mixing.

본 발명에서는 기재로 내열성이 우수한 폴리페닐렌설파이드를 사용하고, 강화재로 고강도의 탄소섬유를, 그리고 내마모성의 향상을 위해 자체윤활성을 가진 흑연분말을 사용하였다. 탄소섬유의 함량은 10중량이하인 경우 순수 폴리페닐렌설파이드의 성형의 어려움을 막아주기는 하나, 제1도의 그래프에 도시한 바와 같이 강화재 첨가의 효과인 강도증가에 큰 영향을 미치지 못하였다. 탄소섬유의 함량이 30중량이상인 경우에는 혼합에 어려움이 있고 혼합된다 하더라도 수지와 섬유간에 균일한 혼합이 일어나지 않아 물성저하의 요인이 되고, 제3도의 그래프에 도시한 바와 같이 마찰계수의 값이 다수 증가하였다. 따라서, 탄소섬유의 배합량은 전체 복합재료에 대해 10-30중량의 범위가 바람직하다. 흑연분말의 함량은 5중량이하인 경우 윤활제 첨가 효과가 두드러지게 나타나지 않고 내마모성 향상의 목적을 달성하기 어렵다. 제5도의 그래프에서 알 수 있는 바와 같이 흑연분말의 함량 증가에 따라 마찰계수가 점차 줄어들고 있다. 흑연분말의 함량이 20중량이상 되면 혼합이 어려워 가공상의 문제점이 생길 뿐만 아니라, 제4도의 그래프에서 알 수 있듯이 강도가 현저히 감소하게 된다.In the present invention, polyphenylene sulfide having excellent heat resistance is used as the substrate, high strength carbon fiber is used as the reinforcing material, and graphite powder having self-lubrication property is used to improve wear resistance. The content of carbon fiber is 10 weight In the following case, the difficulty of forming pure polyphenylene sulfide was prevented, but as shown in the graph of FIG. 1, it did not significantly affect the strength increase effect of the addition of the reinforcing material. 30 weight of carbon fiber In the above case, even if it is difficult to mix, even if mixed, uniform mixing does not occur between the resin and the fiber, which causes a decrease in physical properties, and as shown in the graph of FIG. Therefore, the blending amount of carbon fiber is 10-30 weight based on the total composite material. The range of is preferable. The content of graphite powder is 5 weight In the case of the following, the effect of adding lubricant is not remarkable and it is difficult to achieve the purpose of improving wear resistance. As can be seen in the graph of FIG. 5, the friction coefficient is gradually decreasing as the graphite powder content increases. 20 weight of graphite powder If it is abnormal, not only mixing becomes difficult, but also a processing problem occurs, and as shown in the graph of FIG. 4, the strength is significantly reduced.

따라서, 흑연분말의 함량은 5-20중량가 바람직하다.Therefore, the content of graphite powder is 5-20 weight Is preferred.

[실시예 1]Example 1

기재로 사용한 폴리페닐렌설파이드 수지는 결정성 수지로서 밀도는 1.64g/cm3이고, 열변형온도는 260로서 실제 성형온도는 290-310인 수지를 사용하였다. 강화재로 첨가되는 탄소섬유는 밀도가 1.80g/cm3, 필라멘트의 직경이 5.5μm이고 인장강도는 400kg/mm2인 기본물성을 가지고 있는 것으로, 섬유길이 3mm의 단섬유를 사용하였다. 먼저 폴리페닐렌설파이드를 300로 가열 용융시키고, 폴리페닐렌설파이드와 탄소섬유의 총중량에 대해 탄소섬유의 함량을 0-40중량로 변화시키면서, 기계적으로 혼합하여 사출성형하였다.Polyphenylene sulfide resin used as the substrate is a crystalline resin, the density is 1.64 g / cm 3 , the heat deformation temperature is 260 The actual molding temperature is 290-310 Phosphorus resin was used. Carbon fiber added as a reinforcing material has a basic property of density 1.80g / cm 3 , filament diameter of 5.5μm and tensile strength of 400kg / mm 2 , and short fibers of 3mm fiber length were used. First, polyphenylene sulfide By heating and melting, and the carbon fiber content is 0-40% by weight based on the total weight of polyphenylene sulfide and carbon fiber. Injection molding was carried out by mixing mechanically while changing to.

인장강도와 탄성율의 시험은 만능시험기를 사용하여 행했고, 인장시험의 조건은 상온의 온도에서 1mm/분의 속도로 정했다. 마모시험은 특수강으로 만든 회전하는 원판위에 시험편을 얹고 일정한 압력을 가해 4시간동안 회전시키면서 시험하였다.Tensile strength and modulus were tested using a universal testing machine, and the tensile test conditions were set at a rate of 1 mm / min at room temperature. The abrasion test was carried out by placing the specimen on a rotating disk made of special steel and rotating for 4 hours under constant pressure.

시험결과는 제1도 내지 제3도의 그래프에 나타내었고, 이 시험의 결과로부터 선택된 바람직한 함량인 10-30중량의 탄소섬유를 포함하는 폴리페닐렌설파이드 복합재료의 물성시험 결과를 종래의 유리섬유를 포함하는 나일론 복합재료(비교예 1)의 물성시험결과와 비교하여 표 1에 기재하였다.The test results are shown in the graphs of FIGS. 1 to 3, with a preferred content of 10-30 weight selected from the results of this test. The physical property test results of the polyphenylene sulfide composite material containing carbon fiber of Table 1 are compared with the physical property test results of the conventional nylon composite material containing glass fiber (Comparative Example 1).

[실시예 2]Example 2

기재로 사용한 폴리페닐렌설파이드 수지는 결정성 수지로서, 밀도는 1.64g/cm3이고 열변형온도는 260로서 실제 성형온도는 290-310인 수지를 사용하였고, 강화재로 첨가되는 탄소섬유는 밀도가 1.80g/cm3, 필라멘트의 직경이 5.5μm이고 인장강도는 400kg/mm2인 기본물성을 가지고 있는 것으로, 섬유길이 3mm의 단섬유를 사용하였다. 내마모성 향상을 위해 첨가되는 윤활제로 고체인 흑연분말을 사용하였다. 폴리페닐렌설파이드와 탄소섬유 및 흑연분말의 총중량에 대해 탄소섬유의 함량은 30중량로 고정시킨 후, 흑연분말의 함량을 0-20중량로 변화시키면서 혼합하되, 혼합순서는 먼저 폴리페닐렌설파이드를 300로 가열 용융시키고 흑연분말을 첨가하여 기계적으로 균일하게 혼합한 뒤 다시 탄소섬유를 첨가하여 기계적으로 혼합하였다. 인장강도와 내마모성 시험을 실시예 1과 같은 방법으로 행하여 그 결과를 제4도 및 제5도에 그래프로 도시하였다.Polyphenylene sulfide resin used as the substrate is a crystalline resin, the density is 1.64g / cm 3 and the heat deformation temperature is 260 The actual molding temperature is 290-310 Phosphorus resin was used, and carbon fiber added as reinforcing material had basic properties of density 1.80g / cm 3 , diameter of filament is 5.5μm and tensile strength is 400kg / mm 2 . Used. Solid graphite powder was used as a lubricant added to improve wear resistance. The content of carbon fiber is 30 weight based on the total weight of polyphenylene sulfide, carbon fiber and graphite powder. After fixing to 0, the content of graphite powder is 0-20 While changing the mixture to, but the mixing order is first polyphenylene sulfide 300 The mixture was heated and melted, and the graphite powder was added to mechanically uniformly mix, followed by the addition of carbon fibers and mechanically mixed. Tensile strength and wear resistance tests were conducted in the same manner as in Example 1 and the results are shown graphically in FIGS. 4 and 5.

[비교예 1]Comparative Example 1

비교를 위하여 종래의 나일론 복합재료에 대해서도 물성시험을 행하였다. 나일론 수지로는 나일론 6수지나 나일론 6,6를 사용하였고, 유리섬유의 함량은 10-30중량로 하여 시험하였다. 나일론 수지를 150로 가열용융시키고, 유리섬유의 함량을 10-30중량로 변화시키면서, 기계적으로 혼합하여 사출성형한 후, 실시예 1과 동일한 방법으로 인장강도 탄성율 및 내마모성 시험을 행하여 그 결과를 표 1에 기재하였다.For comparison, a physical property test was also performed on a conventional nylon composite material. Nylon 6 resin or nylon 6,6 was used as the nylon resin, and the content of glass fiber was 10-30 weight. It tested by. Nylon resin 150 By heat melting with a glass fiber content of 10-30 weight After mechanically mixing and injection molding while changing to, the tensile strength modulus and abrasion resistance test were conducted in the same manner as in Example 1, and the results are shown in Table 1.

상기 실시예 및 비교예의 시험결과로부터 알 수 있듯이, 본 발명의 폴리페닐렌설파이드 복합재료는 종래의 나일론 복합재료에 비해 고온에서도 연속사용이 가능할 뿐만 아니라, 높은 인장강도와 우수한 탄성율 및 낮은 마찰계수값, 즉 우수한 내마모성을 갖는다. 또한 사출성형이 가능하여 대량생산할 수 있고, 화학적 분위기에도 내식성이 강해 자동차 부품 및 기타 내마모성이 요구되는 부품에 적용하기에 적합하다.As can be seen from the test results of the examples and comparative examples, the polyphenylene sulfide composite material of the present invention is not only capable of continuous use at a high temperature compared to the conventional nylon composite material, but also has high tensile strength, excellent elastic modulus and low coefficient of friction. That is, it has excellent wear resistance. In addition, injection molding is possible, and mass production is possible, and it is suitable for application to automobile parts and other parts requiring abrasion resistance due to strong corrosion resistance in chemical atmosphere.

Claims (3)

50-85중량의 폴리페닐렌설파이드, 10-30중량의 탄소섬유 및 5-20중량의 흑연분말로 구성되는 자체윤활성을 갖는 폴리페닐렌설파이드 복합재료.50-85 weight Polyphenylene sulfide, 10-30 weight Carbon fiber and 5-20 weight A polyphenylene sulfide composite material having self-lubricating activity composed of graphite powder. 50-85중량의 폴리페닐렌설파이드를 가열용융하고, 5-20중량의 흑연분말을 기계적으로 혼합하여 성형하는 것으로 구성되는 자체윤활성을 갖는 폴리페닐렌설파이드 복합재료의 제조방법.50-85 weight 5-20 weight of the polyphenylene sulfide by heat-melting A method for producing a polyphenylene sulfide composite material having self-lubricating activity comprising mechanically mixing and molding graphite powder. 제2항에 있어서, 상기 성형방법은 사출성형방법인 것을 특징으로 하는 자체윤활성을 갖는 폴리페닐렌설파이드 복합재료의 제조방법.The method of manufacturing a polyphenylene sulfide composite material having self-lubricating activity according to claim 2, wherein the molding method is injection molding.
KR1019950039720A 1995-11-04 1995-11-04 Self lubricating polyphenylene sulfide composite materials and their preparation process KR100217435B1 (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101355472B1 (en) 2010-12-31 2014-01-28 제일모직주식회사 High thermal conductive resin composition
KR101368315B1 (en) * 2010-12-31 2014-02-27 제일모직주식회사 High thermal conductive resin composition including a milled pitch based carbon fiber

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101355472B1 (en) 2010-12-31 2014-01-28 제일모직주식회사 High thermal conductive resin composition
KR101368315B1 (en) * 2010-12-31 2014-02-27 제일모직주식회사 High thermal conductive resin composition including a milled pitch based carbon fiber

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