KR20030005710A - Ultra-High Molecular Weight Polyethylene with Carbon Nanotube and Method the Same - Google Patents

Ultra-High Molecular Weight Polyethylene with Carbon Nanotube and Method the Same Download PDF

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KR20030005710A
KR20030005710A KR1020010041113A KR20010041113A KR20030005710A KR 20030005710 A KR20030005710 A KR 20030005710A KR 1020010041113 A KR1020010041113 A KR 1020010041113A KR 20010041113 A KR20010041113 A KR 20010041113A KR 20030005710 A KR20030005710 A KR 20030005710A
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molecular weight
high molecular
weight polyethylene
ultra
cnt
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KR100454587B1 (en
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임대순
안정욱
주영석
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학교법인고려중앙학원
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    • 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
    • C08K3/041—Carbon nanotubes
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
    • A61F2/00—Filters implantable into blood vessels; Prostheses, i.e. artificial substitutes or replacements for parts of the body; Appliances for connecting them with the body; Devices providing patency to, or preventing collapsing of, tubular structures of the body, e.g. stents
    • A61F2/02—Prostheses implantable into the body
    • A61F2/30—Joints
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L23/04—Homopolymers or copolymers of ethene
    • C08L23/06—Polyethene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2207/00—Properties characterising the ingredient of the composition
    • C08L2207/06—Properties of polyethylene
    • C08L2207/068—Ultra high molecular weight polyethylene

Abstract

PURPOSE: A ultra high-molecular weight polyethylene (UHMWPE) containing carbon nano-tube(CNT) is provided to enhance wear-resistance of the polyethylene by dispersing the polyethylene and CNT in a solvent, then molding the obtained powder after vaporizing the solvent. CONSTITUTION: The UHMWPE containing CNT comprises 0.1 to 0.5 weight parts of CNT based on 100 weight parts of the UHMWPE. The UHMWPE is produced by a process comprising steps of entering the powdery UHMWPE in toluene solvent and dispersing it for 0.5-1 hour by way of ultrasonic treatment; adding 0.1 to 0.5 weight parts of CNT into the dispersed polyethylene based on 100 weight parts of the UHMWPE and dispersing again it for 0.5-1 hour by way of the ultrasonic treatment, then naturally vaporizing the solvent in a hood; and forming the obtained powdery mixture in a mold at 150-200deg.C and the pressure of 20-30MPa for 1-2 hours.

Description

탄소나노튜브가 첨가된 초고분자량 폴리에틸렌 및 그 제조방법{Ultra-High Molecular Weight Polyethylene with Carbon Nanotube and Method the Same}Ultra-High Molecular Weight Polyethylene with Carbon Nanotube and Method the Same}

본 발명은 탄소 나노튜브가 첨가된 초고분자량 폴리에틸렌 및 그 제조방법에 관한 것이며, 더욱 상세하게는 초음파를 사용하여 용매에 녹인 초고분자량 폴리에틸렌과 탄소 나노튜브(CNT)를 잘 분산되도록 하고 그 후에 용매를 증발시켜 얻어진 혼합분말을 몰드(mold)에 넣고 성형시켜 제조하는 탄소 나노튜브가 첨가된 초고분자량 폴리에틸렌 및 그 제조방법에 관한 것이다.The present invention relates to ultra high molecular weight polyethylene to which carbon nanotubes are added, and to a method for preparing the same, and more particularly, to dispersing ultra high molecular weight polyethylene and carbon nanotubes (CNT) dissolved in a solvent using ultrasonic waves. The present invention relates to ultra high molecular weight polyethylene to which carbon nanotubes prepared by putting a mixed powder obtained by evaporation in a mold and forming the same, and a method of manufacturing the same.

종래의 초고분자량 폴리에틸렌(Ultra-High Molecular Weight Polyethylene,UHMWPE)은 일반적인 고분자와 달리 마모특성이 우수하고 생체친화도가 좋으며 상대적인 부피비 질량이 작기 때문에 인체에 이식시키기에는 매우 적절한 물질이었고, 사실상 이러한 기계적 특성을 요구로 하는 인공관절 분야에서 좋은 반응을 얻어왔다. 그러나 초고분자량 폴리에틸렌으로 제조된 인공관절을 시술하고 난 후, 피시술자들에 의해 초고분자량 폴리에틸렌이 마모가 일어난다는 것을 발견하게 되었고, 이러한 마모입자들은 인체의 면역작용에 의해 골흡수(bone resorption)와 골용해(osteolysis)를 유발시켜 인공관절의 수명을 단축시키는 치명적인 요인으로 알려져 있다.Unlike conventional polymers, conventional ultra-high molecular weight polyethylene (UHMWPE) is a very suitable material for implantation into the human body because of its excellent wear characteristics, good biocompatibility, and low relative volume-to-mass ratio. Good response has been obtained in the field of artificial joints requiring. However, after performing artificial joints made of ultra high molecular weight polyethylene, the subjects found that the ultra high molecular weight polyethylene caused abrasion, and these wear particles were subjected to bone resorption and bone by the immune function of the human body. It is known to be a fatal factor that causes osteolysis and shortens the life of artificial joints.

연구자들은 초고분자량 폴리에틸렌의 기계적 특성을 향상시키기 위하여 이온을 주입하는 방법(J. S. Chen 등,Surface and Coatings Technology, 138,33-38 (2001)), 감마선을 조사하여 크로스링킹(crosslinking)을 시키는 방법(G.Lewis, Biomaterials, 22, 371-401 (2001)), 및 섬유를 보강재로 사용하는 방법(J.M. Hofste외, Polymer Bulletin, 36, 213-220 (1996))을 개발하였으나, 현재까지 초고분자량 폴리에틸렌의 내마모성을 향상시키기 위한 인체이식에 적합한 마찰, 마모 특성을 갖는 첨가제는 아직 개발된 바가 없었다.Researchers have used ion implantation to improve the mechanical properties of ultra high molecular weight polyethylene (JS Chen et al., Surface and Coatings Technology, 138,33-38 (2001)), and methods of crosslinking by irradiating gamma rays ( G.Lewis, Biomaterials, 22, 371-401 (2001)), and a method of using fibers as reinforcement (JM Hofste et al., Polymer Bulletin, 36, 213-220 (1996)), but to date, ultra high molecular weight polyethylene Additives with friction and wear properties suitable for human transplantation have not yet been developed to improve wear resistance.

따라서 본 발명자는 초고분자량 폴리에틸렌의 내마모성을 향상시킬 수 있는 첨가제를 개발하여 내마모성이 우수한 초고분자량 폴리에틸렌을 개발하기에 이르렀다.Therefore, the present inventors have developed an additive capable of improving the wear resistance of the ultra high molecular weight polyethylene, thereby leading to the development of the ultra high molecular weight polyethylene having excellent wear resistance.

본 발명의 목적은 인공관절의 연골 대체재료로 사용되고 있는 초고분자량 폴리에틸렌의 내마모성을 향상시키기 위한 첨가제를 제공하기 위한 것이다.An object of the present invention is to provide an additive for improving the wear resistance of ultra high molecular weight polyethylene used as a substitute for cartilage of artificial joints.

본 발명의 다른 목적은 첨가제를 사용하여 내마모성이 향상된 초고분자량 폴리에틸렌의 제조방법을 제공하기 위한 것이다.Another object of the present invention is to provide a method for producing ultra high molecular weight polyethylene with improved wear resistance using additives.

본 발명의 또 다른 목적은 기어, 베어링, 캠, 메카니칼 씰 등과 같이 마모, 마찰 운동을 받는 기계부품으로 사용하기 위한 내마모성이 향상된 초고분자량 폴리에틸렌을 제공하기 위한 것이다.Still another object of the present invention is to provide an ultra high molecular weight polyethylene having improved wear resistance for use as a mechanical part subjected to wear and friction movement, such as gears, bearings, cams, mechanical seals, and the like.

이하, 본 발명의 구성 및 작용을 설명한다.Hereinafter, the configuration and operation of the present invention.

도 1은 본 발명에 따른 탄소나노튜브가 첨가된 초고분자량 폴리에틸렌의 제조방법을 나타낸 공정도이다.1 is a process chart showing a method for preparing ultra-high molecular weight polyethylene with added carbon nanotubes according to the present invention.

도 2는 본 발명에 따른 탄소나노튜브가 첨가된 초고분자량 폴리에틸렌의 마모량을 나타낸 그래프이다.2 is a graph showing the amount of wear of ultra-high molecular weight polyethylene to which carbon nanotubes according to the present invention is added.

본 발명에서 사용되는 탄소 나노튜브(CNT)는 1991년에 발견된 것으로 그래파이트(graphite)가 말려 있는 튜브(tube) 형태로서 탄소 사이의 강한 공유결합에 의해 높은 기계적 강도를 갖고, 높은 영스 모둘러스(Young's modulus)와 높은 종횡비(aspect ratio)로 인하여 매우 우수한 기계적 특성을 나타내는 물질이며, 이러한 특성은 여러 가지 복합체로서 응용될 때 물성 향상을 꾀할 수 있는 잠재적인 가능성이 있다. 그리고 탄소 나노튜브(CNT)는 탄소로 구성되어 있어서 이 물질의 물성에 비해 질량이 매우 낮은 물질이다. 그러므로 다른 첨가제에 의한 초고분자량 폴리에틸렌(UHMWPE)의 기계적 특성 향상을 기대하는 것보다 훨씬 우수한 장점들을 갖추고 있다고 할 수 있다.Carbon nanotubes (CNT) used in the present invention was discovered in 1991, and is a form of a tube in which graphite is rolled, and has high mechanical strength due to strong covalent bonds between carbons, and high Young's modulus ( Because of Young's modulus and high aspect ratio, the material shows very good mechanical properties, and this property has the potential to improve the physical properties when applied as various composites. Carbon nanotubes (CNTs) are made of carbon and are very low in mass compared to their physical properties. Therefore, it can be said that it has much superior advantages than expecting the improvement of the mechanical properties of ultra high molecular weight polyethylene (UHMWPE) by other additives.

탄소 나노튜브(CNT)의 제조방법으로는 전기방전법(arc-discharge), 레이저증착법(laser vaporization), 플라즈마 화학기상증착법(plasma enhanced chemical vapor deposition), 열화학기상증착법(thermal chemical vapor deposition) 등이 있으나, 본 발명에서 사용된 탄소 나노튜브는 대량의 탄소 나노튜브를 합성할 수 있는 열화학기상증착법을 이용하여 합성한다.Carbon nanotube (CNT) manufacturing methods include arc-discharge, laser vaporization, plasma enhanced chemical vapor deposition, and thermal chemical vapor deposition. However, the carbon nanotubes used in the present invention are synthesized using a thermochemical vapor deposition method capable of synthesizing a large amount of carbon nanotubes.

본 발명의 탄소 나노튜브가 첨가된 초고분자량 폴리에틸렌은 내마모성이 향상된 초고분자량 폴리에틸렌으로서 초고분자량 폴리에틸렌(UHMWPE) 100중량부에 대하여 탄소 나노튜브(carbon nanotube, CNT) O.1 내지 0.5중량부를 첨가하여 제조된다.The ultra high molecular weight polyethylene to which the carbon nanotubes of the present invention is added is prepared by adding 0.1 to 0.5 parts by weight of carbon nanotubes (CNT) to 100 parts by weight of ultra high molecular weight polyethylene (UHMWPE) as improved wear resistance. do.

이하에는 첨부된 도면을 참조하여 본 발명의 탄소 나노튜브가 첨가된 초고분자량 폴리에틸렌의 제조방법에 대하여 상세히 설명한다.Hereinafter, with reference to the accompanying drawings will be described in detail a method for producing ultra-high molecular weight polyethylene to which the carbon nanotubes of the present invention is added.

본 발명에 따른 탄소 나노튜브(CNT)가 첨가된 초고분자량 폴리에틸렌의 제조공정을 도 1에 나타내었다.1 shows a manufacturing process of ultra high molecular weight polyethylene to which carbon nanotubes (CNT) are added according to the present invention.

비이커와 같은 용기에 톨루엔과 같은 용매를 넣고, 분말 형태로 존재하는 초고분자량 폴리에틸렌를 넣고, 30분 내지 1시간 정도 초음파를 걸어 초고분자량 폴리에틸렌을 분산시킨다. 용매에 분산된 초고분자량 폴리에틸렌에 탄소 나노튜브(CNT)를 첨가한 후 다시 30분 내지 1시간 정도 초음파를 걸어 탄소 나노튜브(CNT)가 잘 분산되게 한 후, 후드 내에서 용매를 자연증발시킨다. 용매를 증발시킨 후 얻어진 초고분자량 폴리에틸렌과 탄소 나노튜브(CNT) 혼합분말을 몰드(mold)에 넣고 성형시킨다. 성형시 온도는 150 ∼ 200℃, 압력은 20 ∼ 30 MPa로 하는 것이 바람직하며, 성형시간은 1 ∼ 2 시간이 바람직하다. 상기 몰드는사용용도에 따라 여러 가지 형상을 가질 수 있다.A solvent, such as toluene, is placed in a container such as a beaker, ultra-high molecular weight polyethylene is present in powder form, and ultrasonic waves are applied for 30 minutes to 1 hour to disperse the ultra-high molecular weight polyethylene. After adding carbon nanotubes (CNT) to the ultra-high molecular weight polyethylene dispersed in the solvent, and sonicated again for 30 minutes to 1 hour to disperse the carbon nanotubes (CNTs) well, the solvent is naturally evaporated in the hood. After evaporating the solvent, the obtained ultra high molecular weight polyethylene and carbon nanotube (CNT) mixed powder is placed in a mold and molded. It is preferable to make temperature 150-200 degreeC and pressure 20-20 MPa at the time of shaping | molding, and 1 to 2 hours are preferable for shaping | molding time. The mold may have various shapes depending on the intended use.

상기의 방법으로 제조된 탄소 나노튜브(CNT)가 첨가된 초고분자량 폴리에틸렌은 인공관절의 시술부위인 고관절(hip joint), 어깨관절(shoulder joint), 무릎관절(knee joint), 팔꿈치관절(elbow joint), 손목관절(wrist joint) 등의 연골 대체재료에 적용가능하다. 또한, 기어, 베어링, 캠, 메카니칼 씰 등과 같이 마모, 마찰 운동을 받는 기계부품으로 사용되는 고분자 재료에 적용가능하다.The ultra-high molecular weight polyethylene added with carbon nanotubes (CNT) prepared by the above method is a hip joint, a shoulder joint, a knee joint, an elbow joint, which is an artificial joint procedure. ), And can be applied to cartilage substitutes such as wrist joints. It is also applicable to polymer materials used as mechanical parts subjected to wear and friction movement, such as gears, bearings, cams, mechanical seals, and the like.

이하, 본 발명의 구체적인 방법을 실시예를 들어 상세히 설명하고자 하지만 본 발명의 권리범위는 이들 실시예에만 한정되는 것은 아니다.Hereinafter, the specific method of the present invention will be described in detail with reference to Examples, but the scope of the present invention is not limited only to these Examples.

실시예Example

탄소 나노튜브(CNT)가 첨가된 초고분자량 폴리에틸렌(UHMWPE)은 다음과 같이 실시하였다. 100㎖의 비이커에 용매인 톨루엔 30㎖와 분말형태의 초고분자량 폴리에틸렌 5g을 넣은 후, 초음파를 30분동안 가해 초고분자량 폴리에틸렌을 톨루엔에 녹였다. 그 후 초고분자량 폴리에틸렌의 100중량부에 대하여 탄소 나노튜브(CNT)를 각각 O.1중량부, 0.2중량부, 0.5중량부를 첨가하여 다시 초음파를 1시간 동안 가해서 탄소 나노튜브(CNT)가 잘 분산되도록 하였다. 비교 테스트를 위하여 탄소 나노튜브(CNT)가 전혀 첨가되지 않은 초고분자량 폴리에틸렌도 준비하였다.Ultra high molecular weight polyethylene (UHMWPE) added with carbon nanotubes (CNT) was carried out as follows. Into a 100 ml beaker, 30 ml of toluene as a solvent and 5 g of ultra high molecular weight polyethylene in powder form were added, and then ultrasonic waves were added for 30 minutes to dissolve the ultra high molecular weight polyethylene in toluene. Thereafter, 0.1 parts by weight, 0.2 parts by weight, and 0.5 parts by weight of carbon nanotubes (CNT) were added to 100 parts by weight of the ultra high molecular weight polyethylene, and ultrasonic waves were applied for 1 hour, thereby dispersing the carbon nanotubes (CNT) well. It was made. Ultra high molecular weight polyethylene with no carbon nanotubes (CNT) added was also prepared for comparative testing.

그 후 후드 내에서 24시간 동안 자연건조하여 톨루엔을 증발시켰다. 이렇게 얻어진 혼합분말을 금속몰드에 넣고 150℃의 온도, 25MPa 압력으로 1시간 동안 핫프레스(hot press) 한 후 자연냉각하여 탄소 나노튜브(CNT)가 첨가되지 않은 초고분자량 폴리에틸렌와 탄소 나노튜브(CNT)가 각각 0.1중량부, 0.2중량부, 0.5중량부 첨가된 초고분자량 폴리에틸렌을 제조하였다.The toluene was then evaporated by air drying for 24 hours in the hood. The mixed powder thus obtained was put into a metal mold and hot pressed for 1 hour at a temperature of 150 ° C. and 25 MPa pressure, followed by natural cooling, and ultra-high molecular weight polyethylene and carbon nanotubes (CNT) without adding carbon nanotubes (CNT). 0.1 parts by weight, 0.2 parts by weight and 0.5 parts by weight of ultra-high molecular weight polyethylene was added.

상기의 방법으로 얻어진 성형체를 볼 온 디스크(ball on disc) 형태의 마모시험기를 사용하여 마모실험을 하였다. 마모실험은 로드(load)가 5N, 회전속도가 1000rpm, 온도는 상온에서상대재로실리콘 나이트라이드(Si3N4) 볼을 사용하여 2시간 동안 실시하였다.The molded article obtained by the above method was subjected to abrasion test using a wear tester in the form of a ball on disc. Abrasion test was carried out for 2 hours using a silicon nitride (Si 3 N 4 ) ball as a counterpart at a load of 5N, rotational speed of 1000rpm, temperature at room temperature.

실험결과는 도 2에 나타난 바와 같이 탄소 나노튜브(CNT) 첨가량이 증가함에 따라 마모량이 감소하였다. 탄소 나노튜브(CNT)가 0.5중량부 첨가된 시편의 마모량은 탄소 나노튜브(CNT)가 전혀 첨가되지 않은 시편의 마모량에 비해 90% 감소하였다.As shown in FIG. 2, the wear amount decreased as the carbon nanotube (CNT) addition amount increased. The wear amount of the specimen to which 0.5 parts by weight of carbon nanotubes (CNT) was added was reduced by 90% compared to the amount of the specimens to which carbon nanotubes (CNT) were not added.

상기에서 설명한 바와 같이, 본 발명에 따른 탄소 나노튜브(CNT)가 첨가된 초고분자량 폴리에틸렌은 내마모성을 획기적으로 향상시켜 인공관절의 수명을 연장시킬 수 있으며, 또한 본 발명은 기어, 베어링, 캠, 메카니칼 씰 등과 같이 마모, 마찰 운동을 받는 기계부품으로 사용되는 고분자재료에 적용할 수 있는 기계부품산업 및 의료산업상 매우 유용한 발명인 것이다.As described above, the ultra high molecular weight polyethylene added with carbon nanotubes (CNT) according to the present invention can significantly improve the wear resistance to extend the life of artificial joints, and the present invention also provides a gear, bearing, cam, mechanical It is a very useful invention in the mechanical parts industry and the medical industry that can be applied to polymer materials used as mechanical parts subjected to wear and friction movement, such as seals.

Claims (4)

초고분자량 폴리에틸렌(UHMWPE) 100중량부에 대하여 탄소 나노튜브(CNT) O.1 내지 0.5중량부를 첨가하는 것을 특징으로 하는 탄소 나노튜브가 첨가된 초고분자량 폴리에틸렌.Ultra-high molecular weight polyethylene with carbon nanotubes added, characterized in that 0.1 to 0.5 parts by weight of carbon nanotubes (CNT) is added to 100 parts by weight of ultra high molecular weight polyethylene (UHMWPE). 톨루엔 용매에 분말 형태로 존재하는 초고분자량 폴리에틸렌을 넣고 30분 내지 1시간 동안 초음파를 가해 초고분자량 폴리에틸렌를 분산시키는 단계;Adding ultra-high molecular weight polyethylene present in powder form to the toluene solvent and applying ultrasonic waves for 30 minutes to 1 hour to disperse the ultra-high molecular weight polyethylene; 상기 용매에 분산된 초고분자량 폴리에틸렌에 초고분자량 폴리에틸렌 100중량부에 대하여 탄소 나노튜브(CNT) 0.1 내지 0.5중량부를 첨가한 후 다시 30분 내지 1시간 동안 초음파를 가해 탄소 나노튜브가 잘 분산되게 한 후, 후드 내에서 용매를 자연증발시키는 단계; 및After adding 0.1 to 0.5 parts by weight of carbon nanotubes (CNT) to 100 parts by weight of ultra high molecular weight polyethylene dispersed in the solvent, and then ultrasonically applied for 30 minutes to 1 hour to allow the carbon nanotubes to be dispersed well. Spontaneously evaporating the solvent in the hood; And 용매를 증발시킨 후 얻어진 초고분자량 폴리에틸렌과 탄소 나노튜브의 혼합분말을 몰드(mold)에 넣고 150 ∼ 200℃의 온도, 20 ∼ 30 MPa의 압력에서 1∼2시간 동안 성형시키는 단계;Putting the mixed powder of ultra-high molecular weight polyethylene and carbon nanotubes obtained after evaporating the solvent into a mold, and molding the mixture powder for 1 to 2 hours at a temperature of 150 to 200 ° C. and a pressure of 20 to 30 MPa; 로 이루어지는 것을 특징으로 하는 탄소 나노튜브가 첨가된 초고분자량 폴리에틸렌의 제조방법.Method for producing ultra-high molecular weight polyethylene with added carbon nanotubes, characterized in that consisting of. 제 2항의 방법에 의하여 제조되는 것을 특징으로 하는 인공관절.An artificial joint, which is prepared by the method of claim 2. 제 2항의 방법에 의해서 제조되는 것을 특징으로 하는 기계부품.A mechanical part manufactured by the method of claim 2.
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