JP7376513B2 - 組成物、それを用いて形成された被膜、該被膜を有する摺動部材およびその製造方法 - Google Patents
組成物、それを用いて形成された被膜、該被膜を有する摺動部材およびその製造方法 Download PDFInfo
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- JP7376513B2 JP7376513B2 JP2020564959A JP2020564959A JP7376513B2 JP 7376513 B2 JP7376513 B2 JP 7376513B2 JP 2020564959 A JP2020564959 A JP 2020564959A JP 2020564959 A JP2020564959 A JP 2020564959A JP 7376513 B2 JP7376513 B2 JP 7376513B2
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Description
本発明で用いるバインダー樹脂は、耐熱性樹脂として潤滑被膜を形成し、かつ後述する固体潤滑剤を担持するバインダーとしての機能を有する樹脂である。使用することのできる樹脂としては、例えばポリアミドイミド、ポリイミド、エポキシ樹脂、フェノール樹脂、ポリアミド、ポリベンズイミダゾール、ポリフェニルスルフォネートおよびポリエーテルエーテルケトンが挙げられ、これらのうち1以上を含んでいてもよい。好ましくは、バインダー樹脂はポリアミドイミドまたはポリイミドを含有する。さらに好ましくは、バインダー樹脂はポリアミドイミドを含有する。
本発明で用いる硬質粒子は、被膜の耐荷重性を向上させるとともに、耐摩耗性を向上する機能を有するものである。使用することのできる硬質粒子としては、炭化タングステン、炭化チタン、炭化ジルコニウム、酸化ジルコニウム、二硫化タングステン、炭化モリブデン、二ケイ化タングステン、窒化チタンおよび窒化ジルコニウムが挙げられ、これらのうち1以上を含むことができる。本発明で用いる硬質粒子は、少なくとも炭化タングステンを含有する。
本発明で用いる固体潤滑剤は、二硫化モリブデンまたはグラファイトである。固体潤滑剤は被膜の摺動性を向上させる機能を有し、特に二硫化モリブデンとグラファイトは良好な耐摩耗性という摺動特性を有する被膜を形成する観点から本発明の組成物で使用することができる。両者のうちでも、特に摩擦係数を下げ、さらに耐摩耗性を付与する点からグラファイトが好ましい。
本発明の組成物は、塗布性の向上などを目的として溶媒を含有することができる。溶媒はバインダーレジンの種類によって選択することができるが、使用することのできる溶媒としては、例えば、アセトン、メチルエチルケトン、メチルイソブチルケトン、シクロヘキサノン等のケトン類、酢酸メチル、酢酸エチル等のエステル類、トルエン、キシレン等の芳香族炭化水素類、メチルクロロホルム、トリクロロエチレン、トリクロロトリフルオエタン等の有機ハロゲン化合物類、N‐メチル‐2‐ピロリドン(NMP)、N‐エチル‐2‐ピロリドン(NEP)、1,3-ジメチル-2-イミダゾリジノン(DMI)、γ-ブチロラクトン(GBL)、3-メトキシ-N、N-ジメチルプロパンアミド、メチルイソピロリドン(MIP)、ジメチルホルムアルデヒド(DMF)、ジメチルアセトアルデヒド(DMAC)等が挙げられる。これらの溶媒は、1種類または2種類以上の混合溶媒であってもよい。溶媒としては、特にNEP、DMI、GBLおよび3-メトキシ-N、N-ジメチルプロパンアミドが好ましい。
本発明の塗料組成物は、本発明の目的を損なわない限り、さらに必要に応じて、紫外線吸収剤、光安定剤、酸化防止剤、熱重合防止剤、レベリング剤、消泡剤、増粘剤、沈降防止剤、顔料(有機着色顔料、無機顔料)、着色染料、赤外線吸収剤、蛍光増白剤、分散剤、導電性微粒子、帯電防止剤、防曇剤、およびカップリング剤等の1種以上の添加剤を含んでもよい。
本発明の第二の発明は、前述の組成物から作成された被膜に関する。被膜は、前述の組成物を部材表面上に塗布し、その後塗布された組成物を熱硬化させることによって形成される。被膜の形成方法は本発明の第四の発明として後述する。本発明の被膜は、バインダーレジン中に硬質粒子および固体潤滑剤が分散された摺動被膜であり、膜厚は1~50μm、好ましくは5~30μmである。
工程(I)は、(A)バインダー樹脂、(B)硬質粒子、並びに(C)二硫化モリブデンおよびグラファイトからなる群から選択される固体潤滑剤を含有し、硬質粒子として炭化タングステンを含有し、かつ成分(B)と成分(C)の重量比((B)/(C))が1から3の範囲にある組成物を作成する工程である。該組成物は本発明の第一の発明として上述したものである。
工程(II)は、工程(I)にて作成された組成物を部材表面上に塗布する工程である。組成物の塗布方法としては、ディッピング法、スピンコート法、フローコート法、スプレー法、バーコート法、グラビアコート法、ロールコート法、ブレードコート法、スクリーン印刷法およびエアーナイフコート法等を利用することができる。塗膜の厚みは特に限定されるものではないが、1~50μmの厚さが好ましく、5~30μmの厚さがより好ましい。
工程(III)は、工程(II)にて塗布された組成物を熱硬化させることにより、部材表面に潤滑被膜を形成する工程である。熱硬化はオーブンなどによる加熱によって行うことができる。塗布された組成物を熱硬化する際には、一段目の加熱によって組成物中の溶媒を除去し、二段目の加熱によって架橋反応によって硬化させることもできる。例えば、60~100℃で5~30分間一段目の加熱を行い、続いて180~250℃で20~120分間二段目の加熱を行うこともできる。
表1中の「平均粒子径」はレーザー回折散乱法で測定した各粒子の平均粒子径である。
N-エチル-2-ピロリドン(NEP)中で調製された、NEPに溶解したポリアミドイミド樹脂を含むポリアミドイミド樹脂溶液(固形分約35重量%)を用い、ポリアミドイミド樹脂87重量部に対しエポキシ樹脂13重量部となるようにエポキシ樹脂を加え、バインダー樹脂溶液とした。このバインダー樹脂溶液に、バインダー樹脂合計100重量部に対して、粉末状の固体潤滑剤であるグラファイトが55.7重量部となり、硬質粒子である炭化タングステン粒子が127重量部になるように配合し、さらに消泡剤を0.7重量部添加し室温で混合分散した。この混合物を固形分濃度が57重量%になるようにN‐エチル‐2‐ピロリドン(NEP)を用いて希釈し、評価用試験に用いる塗料組成物とした。塗料組成物を円柱状(サイズφ24×7.9mm)のオプティモールインストルメンツブリューテクニックゲーエムベーハー製SRVディスク試験片、材質100Cr6(SUJ2相当)表面にスクリーン印刷版、メッシュ株式会社製を用いて焼成後の膜厚が15±5μmとなるように塗布し、80℃で20分間循環式オーブン中で加熱し溶媒を飛ばした後、220℃で20分間焼成を行い、試験片を得た。
表2または表3に示す量(重量部)の各成分を用いた他は実施例1と同様の操作を行い、各試験片を得た。各実施例および比較例により得られた試験片に対し、後述する耐荷重性(往復摺動試験)を行った結果を合わせて、表2または表3に示した。表2に示すとおり、本発明の実施例にかかる試験片は、比較例に対して、高い焼付きまでの荷重(N)を有するものであった。
SRV摩擦摩耗試験機(オプティモールインストルメンツブリューテクニックゲーエムベーハー製、製品名振動摩擦摩耗試験機 SRV5型)を用い、SRVディスク試験片表面上をSRVシリンダーが往復摺動する方法により耐荷重性を評価した。SRVディスク試験片は直径24mm、高さ7.9mmのオプティモールインストルメンツブリューテクニックゲーエムベーハー製SRVディスク試験片、材質100Cr6(SUJ2相当)を使用し、相手材であるシリンダーはφ15×22mmのオプティモールインストルメンツブリューテクニックゲーエムベーハー製のSRVシリンダー(材質100Cr6(SUJ2相当))を用いた。本発明の組成物からなる被膜が形成されたSRVディスクをSRV5型試験機の試験台に設定し、被膜上にエンジン油(エクソンモービル社製、ガソリン・ディーゼルエンジン専用化学合成油 10W-30 SM/CF)を0.1g滴下した。その後SRVシリンダーを荷重20Nで押し当て、速度30Hz、摺動距離2mm、1分間摺動した後、2分ごとに30Nずつ最大2,000Nまで摺動しながら荷重を上昇させたときの、焼き付き荷重を測定した。具体的には摩擦係数が0.15以上となる前の荷重を焼付き荷重とした。
Claims (12)
- (A)バインダー樹脂、
(B)硬質粒子並びに
(C)グラファイトである固体潤滑剤、を含有する組成物であって、
(B)硬質粒子は、炭化タングステン又は、炭化タングステンと、炭化チタン、炭化ジルコニウム、酸化ジルコニウム、硫化タングステン、炭化モリブデン、二ケイ化タングステン、窒化チタン、窒化ジルコニウム及びアルミナからなる群から選択される1以上との混合物であり、
(A)バインダー樹脂が、ポリアミドイミド、ポリイミド、エポキシ樹脂、およびポリアミド、から選択され、
前記組成物は、(A)バインダー樹脂100重量部に対して、70から140重量部の(B)硬質粒子及び、40から70重量部の(C)固体潤滑剤を含有し、且つ、組成物全体の重量を基準として、10~40重量%の(A)バインダー樹脂を含有し、
成分(B)と成分(C)の重量比((B)/(C))が1から3の範囲にあることを特徴とする、組成物。 - 前記組成物は、組成物全体の重量を基準として、20~30重量%の(A)バインダー樹脂を含有することを特徴とする、請求項1に記載の組成物。
- 前記組成物は、(A)バインダー樹脂100重量部に対して、72から137重量部の(B)硬質粒子及び、50から56重量部の(C)固体潤滑剤を含有することを特徴とする、請求項1又は2に記載の組成物。
- (A)バインダー樹脂が、ポリアミドイミド、エポキシ樹脂、又は、ポリアミドイミド、エポキシ樹脂の混合物である、請求項1~3の何れか一項に記載の組成物。
- (B)硬質粒子は、炭化タングステン又は、炭化タングステンと窒化チタン若しくはアルミナとの混合物である、請求項1~4の何れか一項に記載の組成物。
- 炭化タングステンの含有量が、硬質粒子全体の重量を基準として40重量%以上であることを特徴とする、請求項1~5の何れか一項に記載の組成物。
- レーザー回折散乱法で測定した硬質粒子の平均粒子径が0.1から2.0マイクロメートルである、請求項1に記載の組成物。
- さらに(D)溶媒を含有し、溶媒がN‐エチル‐2‐ピロリドン、1,3-ジメチル-2-イミダゾリジノン、γ-ブチロラクトンおよび3-メトキシ-N、N-ジメチルプロパンアミドから選択される、請求項1に記載の組成物。
- 請求項1~8のいずれか1項記載の組成物から作成された、被膜。
- 請求項1~8のいずれか1項記載の組成物から作成された潤滑被膜を有する、摺動部材。
- 摺動部材がコンプレッサーの斜板、エンジンタペット、カムシャフト、クランクシャフト、エンジンメタル、エンジンピストン、ピストンリング、ギヤ、ドアロック、ブレーキシム、またはブレーキクリップから選択される、請求項10に記載の摺動部材。
- 部材表面上に潤滑被膜を形成する方法であって、次の各工程:
(I)請求項1~8の何れか一項に記載の組成物を作成する工程、
(II)該組成物を部材表面上に塗布する工程、および
(III)塗布された組成物を熱硬化させることにより部材表面に潤滑被膜を形成する工程、
を有する、方法。
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US11180654B2 (en) | 2021-11-23 |
EP3802458A1 (en) | 2021-04-14 |
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KR20210005202A (ko) | 2021-01-13 |
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