KR102628582B1 - 조성물, 조성물로 형성된 필름, 필름을 가지는 활주 부재, 및 그 생산 방법 - Google Patents

조성물, 조성물로 형성된 필름, 필름을 가지는 활주 부재, 및 그 생산 방법 Download PDF

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KR102628582B1
KR102628582B1 KR1020207034369A KR20207034369A KR102628582B1 KR 102628582 B1 KR102628582 B1 KR 102628582B1 KR 1020207034369 A KR1020207034369 A KR 1020207034369A KR 20207034369 A KR20207034369 A KR 20207034369A KR 102628582 B1 KR102628582 B1 KR 102628582B1
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composition
hard particles
weight
binder resin
solid lubricant
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KR1020207034369A
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KR20210005202A (ko
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타까히꼬 사사끼
테쯔지 야마구찌
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듀폰 도레이 스페셜티 머티리얼즈 가부시키가이샤
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Abstract

필름이 (A) 결합제 수지, (B) 경질 입자, 및 (C) 이황화몰리브덴 및 그라파이트로 이루어진 군으로부터 선택된 고체 윤활제를 포함하는 조성물을 사용하여 형성되고, 상기 조성물은 경질 입자로서 텅스텐 탄화물을 포함하고, (B) 경질 입자 및 (C) 고체 윤활제의 중량비((B)/(C))가 1 내지 3의 범위이다.

Description

조성물, 조성물로 형성된 필름, 필름을 가지는 활주 부재, 및 그 생산 방법
본 발명은, 우수한 활주 특성을 갖는 윤활 필름을 제공하는 조성물에 관한 것이다. 또한, 본 발명은 그러한 조성물로 형성된 필름, 그러한 필름을 갖는 활주 부재, 및 그 제조 방법에 관한 것이다.
구성요소 표면의 활주 특성을 개선하기 위한 고체 윤활제를 포함하는 필름-형성 조성물은 산업용 기계, 건설 기계 및 자동차와 같은 다양한 적용예에서 사용된다. 예를 들어, JP2017-201165A는 내연기관용 스커트 부분을 갖는 피스톤을 개시하고, 이는 내부 층 및 외부 층으로 이루어진 2-층 필름을 가지고, 내부 층은 유기 결합제, 고체 윤활제 및 경질 물질 입자를 포함한다. 그러나, 전술한 구조에서, 2-층 필름이 형성되어야 하기 때문에, 제조 단계가 증가되고 복잡해진다. 또한, 유기 결합제, 고체 윤활제, 및 경질 입자를 포함하는 통상적인 필름-형성 조성물로 형성된 윤활 필름은, 더 엄격한 활주 성능이 요구되는 현장에서는 적용되지 못할 수 있다.
JP2017-201165A
본 발명의 목적은, 다양한 산업 분야의 기계 및 자동차에서 이용되는 부재의 표면 상에서 우수한 특성을 갖는 활주 필름을 형성할 수 있는 조성물을 제공하는 것이다.
본 발명자는, 결합제 수지, 고체 윤활제, 및 텅스텐 탄화물을 포함하는 경질 입자를 함유한 조성물을 이용하는 것에 의해서, 더 우수한 활주 성능을 갖는 필름이 형성될 수 있다는 발견을 기초로 본 발명을 고안하였고, 여기에서 고체 윤활제 대 경질 입자의 중량비는 특정 범위 내에서 설정된다.
본 발명의 제1 양태는 (A) 결합제 수지; (B) 경질 입자; 및 (C) 이황화몰리브덴 및 그라파이트로 이루어진 군으로부터 선택된 고체 윤활제를 포함하는 조성물에 관한 것으로서, 상기 조성물은 경질 입자로서 텅스텐 탄화물을 포함하고, (B) 경질 입자 및 (C) 고체 윤활제의 중량비((B)/(C))는 1 내지 3의 범위이다.
본 발명의 제2 양태는 전술한 조성물로 제조된 필름에 관한 것이다.
본 발명의 제3 양태는 전술한 조성물로 제조된 윤활 필름을 갖는 활주 부재에 관한 것이다.
본 발명의 제4 양태는 윤활 필름을 부재의 표면 상에 형성하는 방법에 관한 것으로서, 그러한 방법은: (I) (A) 결합제 수지, (B) 경질 입자, (C) 이황화몰리브덴 및 그라파이트로 이루어진 군으로부터 선택된 고체 윤활제를 포함하는 조성물을 준비하는 단계로서, 상기 조성물은 경질 입자로서 텅스텐 탄화물을 포함하고, (B) 경질 입자 및 (C) 고체 윤활제의 중량비((B)/(C))는 1 내지 3의 범위인, 단계; (II) 조성물을 부재의 표면 상에 도포하는 단계; 및 (III) 도포된 조성물을 열 경화하는 단계로서, 그에 의해서 윤활 필름을 부품의 표면 상에 형성하는, 단계를 포함한다.
본 발명의 조성물에 따라, 특히 내하중성 및 내마모성에서, 통상적인 필름보다 우수한 활주 성능을 갖는 필름을 형성할 수 있다.
(A) 결합제 수지
본 발명에서 이용되는 결합제 수지는, 내열성 수지로서 윤활 필름을 형성하는 수지이고, 후술되는 고체 윤활제를 지지하기 위한 결합제로서의 기능을 갖는다. 이용될 수 있는 수지는, 예를 들어, 폴리아미드이미드, 폴리이미드, 에폭시 수지, 페놀 수지, 폴리아미드, 폴리벤지미다졸, 폴리페닐 설포네이트 및 폴리에테르 에테르 케톤을 포함하고, 이들 중 하나 이상이 함유될 수 있다. 바람직하게, 결합제 수지는 폴리아미드이미드 또는 폴리이미드를 함유한다. 더 바람직하게, 결합제 수지는 폴리아미드이미드를 함유한다.
결합제 수지의 함량은, 전체 조성물의 중량을 기초로, 10 내지 40 중량%, 바람직하게는 20 내지 30 중량%이다.
(B) 경질 입자
본 발명에서 사용되는 경질 입자는 필름의 내하중성을 개선하는 그리고 내마모성을 개선하는 기능을 갖는다. 이용될 수 있는 경질 입자는 텅스텐 탄화물, 티타늄 탄화물, 지르코늄 탄화물, 지르코늄 산화물, 이황화텅스텐, 몰리브덴 탄화물, 이규화텅스텐, 티타늄 질화물 및 지르코늄 질화물을 포함하고, 이들 중 하나 이상이 함유될 수 있다. 본 발명에서 이용되는 경질 입자는 적어도 하나의 텅스텐 탄화물을 함유한다.
텅스텐 탄화물 이외의 다른 경질 입자가 또한 함유될 때, 텅스텐 탄화물의 함량은, 경질 입자의 총 중량을 기초로, 40 중량% 이상인 것이 바람직할 수 있다. 그러한 다른 입자는 가장 바람직하게 티타늄 질화물이다.
본 발명의 경질 입자의 평균 입자 직경은 바람직하게는 0.1 내지 2.0 ㎛, 그리고 특히 바람직하게는 0.1 내지 1.5 ㎛이다. 경질 입자의 평균 입자 직경은 레이저 회절 산란 방법에 의해서 측정될 수 있다.
경질 입자의 함량은 후술되는 고체 윤활제의 배합량에 따라 달라지나, 예로서, 이는 결합제 수지의 100 중량부(parts by weight)에 대해서 70 내지 140 중량부이다.
(C) 고체 윤활제
본 발명에서 사용되는 고체 윤활제는 이황화몰리브덴 또는 그라파이트이다. 고체 윤활제는 필름의 활주 특성을 개선하는 기능을 가지고, 특히, 이황화몰리브덴 및 그라파이트는, 양호한 내마모성의 활주 특성을 갖는 필름을 형성하는 것에 관한 관점에서 본 발명의 조성물에서 이용된다. 둘 중에서, 그라파이트는, 마찰 계수를 감소시키는 그리고 내연마성(abration resistance)을 더 부여하는 것에 관한 관점에서 특히 바람직하다.
고체 윤활제의 함량이 경질 입자의 혼합량에 따라 달라지지만, 예로서, 이는 결합제 수지의 100 중량부에 대해서 40 내지 70 중량부이다.
본 발명의 고체 윤활제의 평균 입자 직경은 레이저 회절 산란 방법에 의해서 측정될 수 있다. 고체 윤활제의 평균 입자 직경은 바람직하게는 0.1 내지 15.0 ㎛, 그리고 특히 바람직하게는 1.0 내지 10.0 ㎛이다.
본 발명에서, 구성요소(B) 대 구성요소(C)의 중량비((B)/(C))는 1 내지 3의 범위 이내인 것이 중요하다. 2개의 성분의 중량비가 1 이상인 경우에, 필름 내에서 내마모성에 기여하는 경질 입자의 비율은 활주 특성에 기여하는 고체 윤활제의 비율보다 커지고, 내마모성 및 내하중성이 크게 개선된다. 특히, 양 성분의 중량비는 바람직하게는 1.2 이상이다. 다른 한편으로, 양 성분의 중량비가 3을 초과하는 경우에, 이는, 마찰 계수가 너무 커지기 때문에, 바람직하지 않다. 더 바람직하게, 2개의 성분의 중량비는 2.5 이하이다.
(D) 용매
본 발명의 조성물은 코팅 특성 및 기타를 개선하기 위한 용매를 함유할 수 있다. 용매는 결합제 수지의 유형에 따라 선택될 수 있다. 이용 가능한 용매는, 예를 들어, 아세톤, 메틸 에틸 케톤, 메틸 이소부틸 케톤 및 시클로헥사논과 같은 케톤; 메틸 아세테이트 및 에틸 아세테이트와 같은 에스테르; 톨루엔 및 자일렌과 같은 방향족 탄화수소; 메틸 클로로포름, 트리클로로에틸렌 및 트리클로로트리플루오로에탄과 같은 유기 할로겐 화합물; N-메틸-2-피롤리돈(NMP), N-에틸-2-피롤리돈(NEP), 1,3-디메틸-2-이미다졸리디논(DMI), γ-부티로락톤(GBL), 3-메톡시-N, N-디메틸프로판아미드, 메틸이소피롤리돈(MIP), 디메틸포름알데히드(DMF), 디메틸아세트알데히드(DMAC) 및 기타를 포함한다. 용매는 하나일 수 있거나 둘 이상이 혼합될 수 있다. 특히 바람직한 용매는 NEP, DMI, GBL 및 3-메톡시-N, N-디메틸프로판아미드이다.
(E) 다른 첨가제
본 발명의 코팅 조성물은, 필요한 경우, 본 발명의 목적을 방해하지 않는 한, 자외선 흡수제, 광 안정화제, 산화 방지제, 열 중합 방지제, 레벨링제(leveling agent), 변형제, 증점제, 침강 방지제(anti-settling agent), 안료(유기 착색 안료, 무기 안료), 착색 염료, 적외선 흡수제, 형광 미백제, 분산제, 전도성 미립자, 대전 방지제, 김서림 방지제, 커플링제(coupling agent) 중 하나 이상을 더 함유할 수 있다.
본 발명의 조성물은 (A) 내지 (C) 그리고 전술한 다양한 선택적 성분을 적절히 혼합하는 것에 의해서 생산될 수 있다.
필름
본 발명의 제2 양태는 전술한 조성물로 제조된 필름에 관한 것이다. 필름은 전술한 조성물을 부재의 표면 상으로 도포하는 것 그리고 이어서 도포된 조성물을 열 경화시키는 것에 의해서 형성된다. 필름을 형성하는 방법을 본 발명의 제4 양태로서 후술할 것이다. 본 발명의 필름은, 경질 입자 및 고체 윤활제가 결합제 수지 내에서 분산된, 활주 필름이고, 필름 두께는 1 내지 50 ㎛, 바람직하게는 5 내지 30 ㎛이다.
본 발명의 제3 양태는 전술한 조성물로 제조된 윤활 필름을 갖는 활주 부재에 관한 것이다. 활주 부재는 압축기의 사판, 엔진 태핏(밸브 상승부), 캠샤프트, 크랭크샤프트, 엔진 금속, 엔진 피스톤, 피스톤 링, 기어, 도어 록, 브레이크 심(brake shim) 또는 브레이크 클립일 수 있다.
본 발명의 제4 양태는 부재의 표면 상에서 윤활 필름을 형성하는 방법이며, 이하의 단계(I) 내지 (III)을 포함한다.
(i) 단계 (I)
단계(I)는 (A) 결합제 수지, (B) 경질 입자, 및 (C) 이황화몰리브덴 및 그라파이트로 이루어진 군으로부터 선택된 고체 윤활제를 포함하는 조성물을 준비하는 단계이고, 상기 조성물은 경질 입자로서 텅스텐 탄화물을 포함하고, (B) 경질 입자 및 (C) 고체 윤활제의 중량비((B)/(C))는 1 내지 3의 범위이다. 상기 조성물은 본 발명의 제1 양태에서 전술한 바와 같다.
(ii) 단계(II)
단계(II)는 단계(I)에서 준비된 조성물을 부재의 표면 상에 도포하는 단계이다. 상기 조성물은 침지, 스핀 코팅, 유동 코팅, 분무, 바 코팅(bar coating), 그라비아 코팅(gravure coating), 롤 코팅, 블레이드 코팅, 스크린 인쇄, 에어 나이프 코팅 및 기타에 의해서 도포될 수 있다. 코팅 필름의 두께는 특별히 제한되지는 않지만, 1 내지 50 ㎛의 두께가 바람직하고, 5 내지 30 ㎛의 두께가 더 바람직하다.
(iii) 단계(III)
단계(III)는, 단계(II)에서 도포된 조성물을 열 경화시키는 것에 의해서 부재의 표면 상에서 윤활 필름을 형성하는 단계이다. 열 경화는 오븐 또는 기타 내에서의 가열에 의해서 실시될 수 있다. 도포된 조성물을 열-경화시킬 때, 조성물 내의 용매가 가열의 제1 페이즈(phase)에서 제거될 수 있고, 조성물은 가열의 제2 페이즈에서 가교결합 반응에 의해서 경화될 수 있다. 예를 들어, 가열의 제1 페이즈는 5 내지 30분 동안 60 내지 100℃에서 실시될 수 있고, 이어서 가열의 제2 페이즈는 20 내지 120분 동안 180 내지 250℃에서 실시될 수 있다.
실시예
본 발명은, 제한적이지는 않지만, 이하의 실시예에 의해서 설명된다. 실시예에서 이용되는 원료 물질이 표 1에 기재되어 있다. 표 1의 "평균 입자 직경"은 레이저 회절 산란 방법에 의해서 측정된 각각의 입자의 평균 입자 직경이다.
[표 1]
실시예 1
N-에틸-2-피롤리돈(NEP) 내에 용해된 폴리아미드이미드 수지를 함유하는 폴리아미드이미드 수지 용액(고체 함량 약 35 중량%)이 NEP 내에서 폴리아미드이미드 수지를 합성하는 것에 의해서 준비되었다. 결과적인 결합제 수지 용액이 87 중량부의 폴리아미드이미드 수지 및 13 중량부의 에폭시 수지를 포함하도록, 에폭시 수지를 폴리아미드이미드 수지 용액에 첨가하였다. 이러한 결합제 수지 용액에서, 결과적인 조성물이 총 결합제 수지의 100 중량부를 기초로 127 중량부의 텅스텐 탄화물 입자 및 55.7 중량부의 그라파이트를 함유하도록, 분말형 고체 윤활제인 그라파이트, 및 경질 입자인 텅스텐 탄화물 입자를 혼합하였고, 이어서 0.7 중량부의 변형제를 더 첨가하였다. 조성물은 상온에서 혼합 및 분산되었다. 혼합물은, 평가 테스트에서 이용되는 코팅 조성물을 만들기 위해서 57 중량%의 고체 함량 농도까지 N-에틸-2-피롤리돈(NEP)으로 희석되었다. 코팅 조성물은, 소성(firing) 후의 필름 두께가 15±5㎛이 되도록, 스크린 인쇄 판(Mesh Corporation)을 이용하는 것에 의해서, SRV 원통형 디스크 테스트 단편(크기: φ24 x 7.9mm, 물질: 100Cr6(SUJ2와 등가) Optimol Instruments Prutechnik GmbH)의 표면 상으로 도포되었고, 용매는 20분동안 80℃에서 순환 오븐 내에서 가열하는 것에 의해서 제거되었다. 그 후에, 소성을 20분 동안 220℃에서 실시하여 테스트 단편을 획득하였다.
실시예 2 내지 8 그리고 비교예 1 내지 5
표 2 또는 표 3에 기재된 성분 및 양(중량부)을 이용하는 것을 제외하고, 실시예 1에서와 동일한 절차를 실시하여 테스트 단편을 획득하였다.
실시예 및 비교예에서 얻어진 테스트 단편에 대해서 후술되는 내하중 테스트(왕복 활주 테스트)를 실시하였고, 결과를 표 2 또는 표 3에 기재하였다. 표 2에 기재된 바와 같이, 본 발명의 실시예에 따른 테스트 단편은, 비교예에 비해서, 큰 포획 하중(load to seizure)(N)을 가졌다.
[표 2]
[표 3]
[평가 방법] 내하중성(왕복 활주 테스트)
SRV 마찰 및 마모 테스트기(Optimol Instruments Prutechnik GmbH, 제품명: oscillation friction and wear tester Model SRV5)를 이용하여, SRV 실린더가 SRV 디스크 테스트 단편의 표면 상에서 왕복되는 방법에 의해서, 내하중성을 평가하였다. SRV 디스크 테스트 단편은 직경이 24 mm였고 높이가 7.9 mm 였고(Optimol Instruments Prutechnik GmbH, 물질: 100Cr6(SUJ2와 등가), 상응 실린더는 φ15 × 22 mm SRV 실린더(Optimol Instruments Prutechnik GmbH, 물질: 100Cr6 (SUJ2와 등가)였다. 본 발명의 조성물로 제조된 필름이 형성된 SRV 디스크를 SRV5 테스터의 테스트 베드 상에 셋팅하였고, 0.1 g의 엔진오일(Exxon Mobil, 가솔린 엔진 및 디젤 엔진을 위해서 화학적으로 합성된 오일 10W-30 SM/CF)을 떨어뜨렸다. SRV 실린더를 20N의 하중으로 프레스하였고, 30Hz의 속력으로 그리고 2 mm의 활주 거리로 1분 동안 활주시킨 후에, 활주시키면서, 매 2분마다 30N만큼 하중을 증가시켜, 포획 하중을 측정하였다. 구체적으로, 마찰계수가 0.15 이상이 되기 전의 하중을 포획 하중으로서 취하였다.

Claims (12)

  1. 조성물로서,
    (A) 결합제 수지;
    (B) 경질 입자; 및
    (C) 이황화몰리브덴 및 그라파이트로 이루어진 군으로부터 선택된 고체 윤활제를 포함하고,
    상기 조성물은 경질 입자로서 텅스텐 탄화물을 포함하고,
    (A) 상기 결합제 수지의 함량이 전체 조성물의 중량을 기초로 10 내지 40 중량%이고,
    (B) 상기 경질 입자의 함량이 (A) 상기 결합제 수지 100 중량부를 기초로 70 내지 140 중량부이고,
    (C) 상기 고체 윤활제의 함량이 (A) 상기 결합제 수지 100 중량부를 기초로 40 내지 70 중량부이고,
    (B) 상기 경질 입자 및 (C) 상기 고체 윤활제의 중량비((B)/(C))가 1.46 내지 2.47의 범위인, 조성물.
  2. 제1항에 있어서,
    상기 고체 윤활제가 그라파이트인, 조성물.
  3. 제1항에 있어서,
    상기 경질 입자가, 텅스텐 탄화물에 더하여, 티타늄 탄화물, 지르코늄 탄화물, 지르코늄 산화물, 이황화텅스텐, 몰리브덴 탄화물, 이규화텅스텐, 티타늄 질화물 및 지르코늄 질화물로 이루어진 군으로부터 선택된 적어도 하나를 더 포함하고, 상기 조성물이 연질 금속 입자를 포함하지 않는, 조성물.
  4. 제3항에 있어서,
    상기 텅스텐 탄화물의 함량은 경질 입자의 총 중량을 기초로 40 중량% 이상인, 조성물.
  5. 제1항에 있어서,
    상기 결합제 수지가 폴리아미드이미드, 폴리이미드, 에폭시 수지, 페놀 수지, 폴리아미드, 폴리벤지미다졸, 폴리페닐 설포네이트 및 폴리에테르 에테르 케톤으로 이루어진 군으로부터 선택되는, 조성물.
  6. 제1항에 있어서,
    결합제 수지로서 폴리아미드이미드를 포함하는, 조성물.
  7. 제1항에 있어서,
    레이저 회절 산란 방법에 의해서 측정된 상기 경질 입자의 평균 입자 직경이 0.1 내지 2.0 마이크로미터인, 조성물.
  8. 제1항에 있어서,
    (D) 용매를 더 포함하고, 상기 용매는 N-에틸-2-피롤리돈, 1,3-디메틸-2-이미다졸리디논, γ-부티로락톤, 및 3-메톡시-N, N-디메틸프로판아미드로 이루어진 군으로부터 선택되는, 조성물.
  9. 제1항 내지 제8항 중 어느 한 항의 조성물로 제조된 필름.
  10. 제1항 내지 제8항 중 어느 한 항의 조성물로 제조된 윤활 필름을 갖는 활주 부재.
  11. 제10항에 있어서,
    상기 활주 부재가 압축기의 사판, 엔진 태핏, 캠샤프트, 크랭크샤프트, 엔진 금속, 엔진 피스톤, 피스톤 링, 기어, 도어 록, 브레이크 심 또는 브레이크 클립인, 활주 부재.
  12. 윤활 필름을 부재의 표면 상에 형성하기 위한 방법으로서,
    (I) (A) 결합제 수지, (B) 경질 입자, 및 (C) 이황화몰리브덴 및 그라파이트로 이루어진 군으로부터 선택된 고체 윤활제를 포함하는 조성물을 준비하는 단계로서, 상기 조성물은 상기 경질 입자로서 텅스텐 탄화물을 포함하고, (A) 상기 결합제 수지의 함량이 전체 조성물의 중량을 기초로 10 내지 40 중량%이고, (B) 상기 경질 입자의 함량이 (A) 상기 결합제 수지 100 중량부를 기초로 70 내지 140 중량부이고, (C) 상기 고체 윤활제의 함량이 (A) 상기 결합제 수지 100 중량부를 기초로 40 내지 70 중량부이고, (B) 상기 경질 입자 및 (C) 상기 고체 윤활제의 중량비((B)/(C))가 1.46 내지 2.47의 범위인, 단계;
    (II) 상기 조성물을 부재의 표면 상에 도포하는 단계; 및
    (III) 상기 도포된 조성물을 열-경화시키고, 그에 의해서 윤활 필름을 상기 부재의 표면 상에 형성하는 단계를 포함하는, 방법.
KR1020207034369A 2018-06-11 2019-05-31 조성물, 조성물로 형성된 필름, 필름을 가지는 활주 부재, 및 그 생산 방법 KR102628582B1 (ko)

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