JP7417916B2 - 炭素移着膜が形成された摺動部材 - Google Patents
炭素移着膜が形成された摺動部材 Download PDFInfo
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- JP7417916B2 JP7417916B2 JP2018209298A JP2018209298A JP7417916B2 JP 7417916 B2 JP7417916 B2 JP 7417916B2 JP 2018209298 A JP2018209298 A JP 2018209298A JP 2018209298 A JP2018209298 A JP 2018209298A JP 7417916 B2 JP7417916 B2 JP 7417916B2
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Classifications
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
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Description
上記第1部材の摺動面と上記第2部材の摺動面の間に、上記炭素を含む潤滑材料を適用する潤滑材料適用工程と、
上記第1部材の摺動面と上記第2部材の摺動面を相対的に摺動させて、上記第2部材に由来する炭素を上記第1部材表面に移着させることにより、上記第1部材表面に炭素移着膜を形成する移着膜形成工程とを少なくとも備える、
炭素移着膜が形成された摺動部材の製造方法(以下、「本発明の炭素移着膜が形成された摺動部材の製造方法」と称する場合がある)を提供する。
以下本発明を、図面を参照しつつ詳細に説明する。図1は本発明の炭素移着膜が形成された摺動部材1の一例の拡大模式図である。摺動部材を構成する基材3aの表面に、炭素移着膜2が形成されている。本発明の炭素移着膜が形成された摺動部材1は、基材3aの表面にsp2結合を有する炭素と、sp3結合を有する炭素を含む炭素移着膜2が形成されている。
上記基材3aとしては、特に限定されず、例えば、炭素鋼、クロム鋼、クロムモリブデン鋼などの合金鋼、合金工具鋼、ステンレス鋼(例えば、SUS)、軸受鋼(例えば、SUJ)、バネ鋼(例えば、SUP)などの特殊用途鋼などの金属材であってもよい。また上記基材表面は、ダイヤモンドライクカーボン(DLC)膜が成膜されていてもよいし、めっき、化成処理、陽極酸化などの各種電気化学処理;流動性塗装や粉体塗装などの各種塗装;ショットブラストなどの物理的表面処理;といった各種の表面処理が行われていてもよい。
上記炭素移着膜2は、上記基材3aの表面に形成されている。本明細書において「表面」とは、種々の摺動部材の可動部における摺動面を指す。また本明細書において「移着膜」とは、相対的に摺動する2つの部材の少なくとも一方から生じた摩耗粉(移着粒子とも呼ぶ)が、他方の部材の表面に付着することにより形成された被膜や、潤滑材料に含まれる添加剤や摩耗粉が摺動面に吸着すること又は化学反応によって形成された被膜(いわゆる、トライボフィルム)を含む概念である。
測定機器:レーザーラマン分光光度計 商品名「NRS-5100」(日本分光株式会社製)
測定光源:532nm
出力 :0.8mW
スリット幅:100×1000mm
露光時間:10秒
積算回数:4回
測定機器:エネルギー分散型X線分光分析装置 商品名「X-Max50」(OXFORD instrumests製)
加速電圧:5kV
本明細書において、炭素を含む潤滑材料4とは、摺動面に、摺動に適したなじみ面(低摩擦面)を形成させるための初期なじみ剤と、摩擦や摩耗を低減させる目的で用いられる一般的な潤滑剤の双方を含む概念である。上記炭素を含む潤滑材料4は、潤滑基剤と種々の潤滑特性(耐摩耗、摩擦低減など)を付与する炭素を含有する添加剤から構成される。
上記ND粒子は、特に限定されず、公知ないし慣用のND粒子を用いることができる。上記ND粒子は、表面修飾されたND(表面修飾ND)粒子であっていてもよいし、表面修飾されていないND粒子であってもよい。なお、表面修飾されていないND粒子は、表面にヒドロキシル基(-OH)を有する。上記ND粒子は、一種のみを用いてもよいし二種以上を用いてもよい。
本発明の炭素移着膜が形成された摺動部材の製造方法は、第1部材と第2部材を、炭素を含む潤滑材料を介して、相対的に摺動させて炭素移着膜が形成された摺動部材を製造する方法であって、上記第1部材の摺動面と上記第2部材の摺動面の間に、炭素を含む潤滑材料を適用する潤滑材料適用工程と、上記第1部材の摺動面と上記第2部材の摺動面を相対的に摺動させて、上記第2部材に由来する炭素を上記第1部材表面に移着させることにより、上記第1部材表面に炭素移着膜を形成する移着膜形成工程とを少なくとも備える、炭素移着膜が形成された摺動部材の製造方法である。
上記潤滑材料適用工程は、上記第1部材の摺動面と上記第2部材の摺動面の間に、炭素を含む潤滑材料を適用する工程である。
上記移着膜形成工程は、上記第1部材の摺動面と上記第2部材の摺動面を相対的に摺動させて、上記第2部材に由来する炭素を上記第1部材表面に移着させることにより、上記第1部材表面に炭素移着膜を形成する工程である。
下記工程を経て、炭素を含む潤滑材料を製造した。
得られたND水分散液のナノダイヤモンド含有量(ND濃度)は、秤量した分散液3~5gの当該秤量値と、当該秤量分散液から加熱によって水分を蒸発させた後に残留する乾燥物(粉体)について精密天秤によって秤量した値とに基づき、算出した。
得られたND水分散液に含まれるナノダイヤモンド粒子の粒径(メディアン径、D50ないしD90)は、Malvern社製の装置(商品名「ゼータサイザー ナノZS」)を使用して、動的光散乱法(非接触後方散乱法)によって測定した。測定に付されたND水分散液は、固形分濃度ないしナノダイヤモンド濃度が0.5~2.0質量%となるように超純水で希釈された後に超音波洗浄機による超音波照射を経たものである。
得られたND水分散液のpHは、pH試験紙(商品名「スリーバンドpH試験紙」、アズワン株式会社製)を使用して測定した。
得られたND水分散液に含まれるナノダイヤモンド粒子のゼータ電位は、Malvern社製の装置(商品名「ゼータサイザー ナノZS」)を使用して、レーザードップラー式電気泳動法によって測定した。測定に付されたND水分散液は、固形分濃度ないしナノダイヤモンド濃度が0.2質量%となるように超純水で希釈された後に超音波洗浄機による超音波照射を経たものであり、ゼータ電位測定温度は25℃である。
上述の酸素酸化処理後、及び、水素還元処理後のナノダイヤモンド試料のそれぞれについて、FT-IR装置(商品名「Spectrum400型FT-IR」,株式会社パーキンエルマージャパン製)を使用して、フーリエ変換赤外分光分析(FT-IR)を行った。本測定においては、測定対象たる試料を真空雰囲気下で150℃に加熱しつつ赤外吸収スペクトルを測定した。真空雰囲気下の加熱は、エス・ティ・ジャパン社製のModel-HC900型Heat ChamberとTC-100WA型Thermo Controllerとを併用して実現した。
上記で得られたND水分散液と、潤滑基剤である超純水とを混合して濃度調整することで、炭素を含む潤滑材料A(表面にカルボキシル基を有するND粒子0.001質量%含有水溶液)を作成した。
炭素移着膜が形成された摺動部材の作成には、ロードセル59を備える滴下型ボールオンディスク型すべり摩擦試験機5(図3)を用いた。直径8mmのSUS304製のボール51(以下「SUSボール」と称する場合がある)を第1部材とし、a-C:H膜(約3μm)を摺動面に成膜した直径30mm,厚さ4mmのSUJ2製のディスク53(以下「DLCディスク」と称する場合がある)を第2部材として用いた。試験開始時に上記第2部材表面の摺動面(すなわち、上記第1部材の摺動面と上記第2部材の摺動面の間)に炭素を含む潤滑材料Aを1mL滴下し、室温にて摺動させた。摺動条件は、すべり速度10mm/s、荷重10N、すべり距離100mとした。これにより、第1部材の摩耗痕上に炭素移着膜が形成され、第1部材の基材表面に炭素移着膜が形成された摺動部材を得た。
炭素を含む潤滑材料B(表面にカルボキシル基を有するND粒子0.01質量%含有水溶液)を用いた以外は、上記実施例1と同様に実施し、実施例2の炭素移着膜が形成された摺動部材を得た。
炭素を含む潤滑材料C(表面にカルボキシル基を有するND粒子0.1質量%含有水溶液)を用いた以外は、上記実施例1と同様に実施し、実施例3の炭素移着膜が形成された摺動部材を得た。
潤滑材料としてND粒子を含まない水(超純水)を用いた以外は、上記実施例1と同様に実施し、比較例の摺動部材(SUSボール)を得た。
上記実施例1において、試験開始から終了までの摩擦係数の変化を測定し、低摩擦効果の評価を行った。すなわち、炭素移着膜が形成された摺動部材を得る工程中の、摩擦低減効果の変化を評価した。結果を図4に示す。
上記試験1の終了後、次の手順にて摩耗量を測定した。実施例1及び比較例1の各摺動部材表面のボール摩耗痕の画像を共焦点レーザー顕微鏡(商品名「OPTELICS H1200」、レーザーテック株式会社製)にて取得し、摩耗痕を新円に近似することで摩耗痕半径を算出した。ここで、ボール半径をR(mm)、摩耗痕半径をr(mm)、摩耗高さをh(mm)とする。画像から算出して得た摩耗痕半径から下記式(1)により摩耗高さを算出する。なお、下記式(1)におけるRは、上記摺動部材(SUSボール)の半径であって、4(mm)である。
炭素移着膜の分析は、水との接触角、ラマン分光分析、走査型電子顕微鏡―エネルギー分散型X線分光分析(SEM EDS)、及び算術平均表面粗さ(Ra)によって行った。なお比較例1では、摺動部材(SUSボール)の摺動表面を評価した。
試験1を終了した試料表面に、水を液量5μL滴下し、接触角計(商品名「極小接触角計MCA-3」、協和界面化学株式会社製)を用いて、その際の表面と液滴の角度を画像から取得した。結果を図5、図6に示す。
試験1を終了した試料表面に、レーザーラマン分光光度計(商品名「NRS-5100」、日本分光株式会社製)を用いて次の測定条件で照射した。結果を図7に示す。
測定光源:532nm
出力 :0.8mW
スリット幅:100×1000mm
露光時間:10秒
積算回数:4回
試験1を終了した試料表面を、エネルギー分散型X線分光分析装置(商品名「X-Max50」、OXFORD instruments製)を用いて、加速電圧5kVの条件で測定した。結果を図8、図9に示す。また表面性状(SEM像)も観察した。
試験1を終了した試料表面について、走査型プローブ顕微鏡(商品名「E-sweep」、日立ハイテクサイエンス製)を用いJIS B 0601:2013に従って、算術平均表面粗さ(Ra)を測定した。なお、測定は摺動時のすべり方向に対して、平行方向、垂直方向のそれぞれの向きに対して行った。結果を図10に示す。
実施例1~3の各摺動部材について試験1を実施した。次いで、得られた摩擦係数の変化に基づいて、2回目のなじみが発生するまでのすべり距離に及ぼす、上記第2部材の摺動痕単位面積あたりの、炭素を含む潤滑材料に含まれるND粒子数の影響を評価した。試験1では、上記第1部材の摺動面と上記第2部材の摺動面の間に、炭素を含む潤滑材料A~C、1mLを滴下すると、摩擦により上記第2部材の摺動痕上に均一に分布するため、滴下した炭素を含む潤滑材料A~Cに含まれるND粒子数(濃度)を、上記第2部材の摺動痕面積で除することにより、摺動痕単位面積あたりのND粒子数を得ることができる。なお、炭素を含む潤滑材料A~C、1mL中に含まれるND粒子数は、ND粒子径を5nm、密度3.2g/cm3として算出した。結果を図11に示す。
図4に、比較例1(図中、C1と示す)として水中、実施例1(図中、E1として示す)として炭素を含む潤滑材料A(ND粒子0.01質量%含有水溶液)中における典型的な摩擦特性と第1部材(SUS304製ボール)の摩耗曲線に示す。ND粒子を含む炭素を含む潤滑材料Aを添加することにより摩擦係数は0.06から0.03に半減した。また、低摩擦効果はすべり距離100mにおいて維持されていた。
2 炭素移着膜
3a 基材
3b 第1部材
3c 第2部材
4 炭素を含む潤滑材料
5 滴下型ボールオンディスク型すべり摩擦試験機
50 ベース
51 SUSボール
52 ボールホルダー
53 DLCディスク
54 ディスクホルダー
55 モーター
56 荷重
57a,b ベアリング
58 ピボット
59 ロードセル
Claims (5)
- 基材表面に、sp2結合を有する炭素と、sp3結合を有する炭素を含む炭素移着膜が形成され、
前記炭素移着膜における、前記sp2結合を有する炭素と前記sp3結合を有する炭素の和に対する、前記sp3結合を有する炭素の比率sp3/(sp2+sp3)は、0.5以上であり、
前記炭素移着膜は、532nmの測定光源を用いたラマン分光分析によって得られるラマンスペクトルにおいて、1570~1640cm-1の範囲に観測されるGバンドのピークと、1300~1400cm-1の範囲に観測されるDバンドのピークを有し、
前記比率sp3/(sp2+sp3)は、前記Dバンドのピーク面積強度(Id)と前記Gバンドのピーク面積強度(Ig)の和に対する、Dバンドのピーク面積強度(Id)の比率Id/(Id+Ig)であり、
前記炭素移着膜における炭素含有量は20原子質量%以上であり、
前記炭素移着膜の算術平均表面粗さ(Ra)が30nm以下である、摺動部材。 - 前記炭素移着膜の膜厚が100~1000nmである、請求項1に記載の炭素移着膜が形成された摺動部材。
- 基材表面に、sp2結合を有する炭素と、sp3結合を有する炭素を含む炭素移着膜が形成され、
前記炭素移着膜における、前記sp2結合を有する炭素と前記sp3結合を有する炭素の和に対する、前記sp3結合を有する炭素の比率sp3/(sp2+sp3)は、0.5以上であり、
前記炭素移着膜は、532nmの測定光源を用いたラマン分光分析によって得られるラマンスペクトルにおいて、1570~1640cm-1の範囲に観測されるGバンドのピークと、1300~1400cm-1の範囲に観測されるDバンドのピークを有し、
前記比率sp3/(sp2+sp3)は、前記Dバンドのピーク面積強度(Id)と前記Gバンドのピーク面積強度(Ig)の和に対する、Dバンドのピーク面積強度(Id)の比率Id/(Id+Ig)である摺動部材を製造する方法であり、
第1部材と第2部材を、炭素を含む潤滑材料を介して、相対的に摺動させて炭素移着膜が形成された摺動部材を製造する方法であって、
前記第1部材の摺動面と前記第2部材の摺動面の間に、前記炭素を含む潤滑材料を適用する潤滑材料適用工程と、
前記第1部材の摺動面と前記第2部材の摺動面を相対的に摺動させて、前記第2部材に由来する炭素を前記第1部材表面に移着させることにより、前記第1部材表面に炭素移着膜を形成する移着膜形成工程とを少なくとも備え、
前記炭素を含む潤滑材料がナノダイヤモンド粒子を含み、
前記第2部材が前記第1部材との摺動面にダイヤモンドライクカーボン膜を有する、炭素移着膜が形成された摺動部材の製造方法。 - 前記第1部材が、金属材である、請求項3に記載の炭素移着膜が形成された摺動部材の製造方法。
- 境界潤滑条件下で、前記潤滑材料適用工程と前記移着膜形成工程を行う請求項3又は4に記載の炭素移着膜が形成された摺動部材の製造方法。
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