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1 Boundary Lubrication Mechanism for Self-lubricating ecialty Steel with Low Friction Loss Kunichika Kubota Seishin Ueda Tatsuya Shoji The Hitachi-developed steel SLD-MAGIC TM has become popular in the Japanese die and mold market for cold-working processes because it exhibits superior galling resistance to other steel and iron materials. However, until recently, the nanoscale mechanism responsible for its lubrication properties has not been well understood. To clarify this issue, samples of different types of steel were analyzed using ball-on-disk tribometry, X-ray photoelectron spectroscopy, Raman spectroscopy, and X-ray fluorescence spectroscopy using synchrotron radiation. The results led to the development of a new boundary lubrication model, referred to as the CCSC model. This report describes the foundations of this model and its tribological implications.
2 低フリクションを実現する自己潤滑性特殊鋼の境界潤滑機構 潤滑における機械損傷のメカニズムを説明できる 4 本報 保持時間 秒以下で摩擦係数が特に低く Cu と S を同 告では そのモデルの創出過程と展望について報告する 時添加したものは良好な特性を示していることが分かっ た 2 図 2 は図 1 の JIS 2. 実験方法 と SLD-MAGIC だけの摩擦 係数の時間変化を抜き出したものである この中で 摺動 表 1 に評価装置および条件を示す 摩擦係数計測用の試 を 1 秒間行った摩擦ありと摩擦なしの表面分析を で 験機は ASTM G99 相当のボールオンディスク試験機で 行った 図 3 にその結果を示す 表面は炭素のコンタミ ディスク側をテストピースとし ボールは直径 6 mm の ネーションが多いが Ar スパッタを進めると徐々に SUJ2 62HRC を用いた は島津製作所製μ -ESCA O のピークが上がった しかし Cu と S は検出されなかっ AXIS 放 射 光 は J-Park KEK-PF た 日立専用ライン BL-11B ラマン分光法は日本電子製 JRS-SYS を用いた 表 2 には実験に用いた合金組成を示す 油の吸着は 図 1 の状態は無洗浄でのテストを行い 図 1 では油を塗布して 表 2 供試材の化学組成 Table 2 Chemical compositions of samples 布で拭きとっていたが それ以降のデータ に 関 し て は 1. C 8.3%Cr Ni Mo W Al Cu S Eppendorf 社製精密ピペット 1- μ l を用い アセト 1.5%C 12.%Cr Mo V 8%Cr steel 1.%C 8.3%Cr Mo V -Cu 1.%C 8.3%Cr Ni Mo W Al S -S 1.%C 8.3%Cr Ni Mo W Al Cu -Al 1.%C 8.3%Cr Ni Mo W Cu S 表 1 評価装置および条件 Table 1 Analysis methods and conditions Name of Manufacturer equipment or place Details of conditon Ball on disk Nanotec (Japan) ball; 6 mm SUJ2 (AISI 52) 62HRC, radius of friction track; 2.89 mm, pressure; 8 MPa, velocity; 11 m/min, disk specimen; mm 5 t (Ra;.2 μm), equivalent to AISI G99 analysis Shimazu μ-esca AXIS 15 kev target; Al2O3 Synchrotron radiation J-PARC KEK-PF, exclusive line of Hitachi BL-11B Raman analysis JOEL JRS-SYS (infared wavelength; 633 nm) Without friction -Cu (61.6) Kinetic friction coefficient.6 8%Cr (63.1) (61.1) Stage1.4.3 m With friction.6 Kinetic friction coefficient ン希釈により精密な付着量の管理を行った Stage2 8 1 Holding time (sec) -S (61.4).2 (61.4).1 図 2 と の 分析結果 Fig. 2 Frictional behavior of samples used for analysis -Al (61.4) 8 1 with friction with friction Holding time (sec) C content (atomic%) 3. 1 SLD-MAGIC の摩擦特性 合金元素の影響 Cu と S の効果 7 O content (atomic%) 3. 実験結果 25 content (atomic%) 図 1 摩擦挙動に作用する合金元素 内数字は硬さ HRC Fig. 1 Effect of alloying elements on frictional behavior (numbers in parentheses show hardness (HRC) of disk specimens) 3 1 図 1 は合金実験により確かめられた摩擦挙動に作用す る金属元素を示す 本実験では 自己潤滑性に有効と思わ れる元素を SLD-MAGIC から抜いて実験を行った 意図 的脱脂が行われていないこれらの結果より -Al SLDMAGIC から Al を抜いた組成 開発鋼 SLD-MAGIC のみ uttering depth (nm) 図 3 最表面から 3 nm の深さまでの元素分布 Fig. 3 Composition profiles from top surface to 3 nm depth 日立金属技報 Vol
3 との摩擦面の違い 自然酸化物の形成 状況 両者とも O のピークが高いので最表面の酸化物構造は O 主体であることが分かる また 摩擦ありの 図 4 にはスパッタしなかった場合の による の は安定酸化物のピークが弱まり 水酸化物のピークが高く 2p 軌道のピークを示す 信号強度の違いはあるもののケ なっていることから 酸化膜の奥は水酸化物状態になって ミカルシフトは見られず 鋼種 摩擦あり / なしの化学結 いることが分かる 一方 摩擦ありの開発鋼のピークは 合状態の差異は見られなかった 次に 3 nm スパッタし 安定酸化物のピークの発達が著しいことから O が安 た場合の の 2p 軌道のピークを図 5 に示す 定酸化物へ変質したことがうかがえる ここでは摩擦ありの にのみ金属 のピークが 以上の結果を図 7 にまとめた 開発鋼には酸化膜の損 見られ その他のものは 酸化膜のピークのみであった 傷は認められないが 不安定な酸化物が摩擦により安定酸 つまり 図 2 中に示すように 摩擦係数が上昇していた 化物へ変質している 一方 では酸化膜が約 2 nm のほうが酸化膜が摩耗で薄くなっていたため 3 程度損傷を受けた状態になっており これが 摩擦係数が nm 掘り進んだことにより のみが金属新生面がむ 上がる原因であることが分かる ただし 摩擦界面上のい き出しになっていることを示している 図 6 はスパッタし かなる現象によって開発鋼の自然酸化膜が損傷しなかった なかった場合の O-1s ピークであるが 水酸化物 OOH のかは依然として不明であった 安定酸化物 2O3 or 3O4 O の 3 つのケミカルシフ トが検出された 摩擦されていないほうは開発鋼 p3/2/1 2p3/2/1 2p3/2/1 2p3/2/1 with friction without friction O O O O 1s/1 1s/1 1s/1 1s/1 O binding energy 9 with friction OOH binding energy 8 7 with friction 1 with friction Binding energy (ev) 7 Binding energy (ev) 図 6 スパッタなしの O-1s 軌道ピーク Fig. 6 O-s1 spectrum before sputtering 図 4 スパッタなしの -2p 軌道ピーク Fig. 4-2p spectrum before sputtering before sliding /data/an9_s2 /data/an9_s3 /data/an9_m2 /data/an9_m3 Intensity (%) O3 and 3O4 binding energies Intensity (%) Intensity (%) /data/an9_s2 /data/an9_s3 /data/an9_m2 /data/an9_m3 /data/an9_s2 /data/an9_s3 /data/an9_m2 /data/an9_m3 2p3/2/3 2p3/2/3 2p3/2/3 2p3/2/3 a 2O3 or 3O4 with friction with friction O The thickness of both samples is more than 5 nm at the beginning oxide binding energy pure binding energy OOH b 735 after sliding WEAR The thickness of sample has became less than 3 nm after sliding 7 Binding energy (ev) TM 図 5 3 nm スパッタした場合の -2p 軌道ピーク Fig. 5-2p spectrum after 3 nm sputtering 22 日立金属技報 Vol 図 7 分析結果の模式図 a SLD-MAGIC b Fig. 7 Schematic illustration of sliding wear test based on TM results (a) SLD-MAGIC (b)
4 Fig. 8 Synchrotron radiation results for SLD-MAGIC TM and SDK11 (a) electron yield (EY) (b) X-ray fluorescence yield (FY) Fig. 9 Differential EY and FY values for SLD-MAGIC TM Fig. 1 Results of ball-on-disk tests with (OA) and without (FR) turbine oil adsorption 23
5 Fig. 12 Schematic drawing of crystal structure of H 2SO 4-GIC Fig. 11 Raman spectra from frictional surfaces for the case of oil adsorption (a) SLD-MAGIC TM (b) I II Fig. 13 Double quasi ternary phase diagram illustrating CCSC model 24
6 Fig. 14 Dependence of lifespan up to friction coefficient of.3 on amount of oil Fig. 15 Results of friction tests in the presence of fromic acid and acetic acid in parafin (amount of oil;.1 mm 3, SK5; AISI W1-8) 25
7 Fig. 16 Schematic drawing of Stribeck curve 26
8 Kunichika Kubota Seishin Ueda Tatsuya Shoji 27
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