JP2024075109A - Coated Cutting Tools - Google Patents
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- 150000004767 nitrides Chemical class 0.000 claims abstract description 58
- 238000000576 coating method Methods 0.000 claims abstract description 44
- 239000011248 coating agent Substances 0.000 claims abstract description 43
- 229910008484 TiSi Inorganic materials 0.000 claims abstract description 30
- 238000002441 X-ray diffraction Methods 0.000 claims abstract description 19
- 239000000758 substrate Substances 0.000 claims abstract description 17
- 229910052751 metal Inorganic materials 0.000 claims abstract description 7
- 229910052752 metalloid Inorganic materials 0.000 claims abstract description 7
- 150000002738 metalloids Chemical class 0.000 claims abstract description 7
- 229910052755 nonmetal Inorganic materials 0.000 claims abstract description 5
- 230000001747 exhibiting effect Effects 0.000 claims description 2
- 238000004544 sputter deposition Methods 0.000 abstract description 19
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 21
- 229910045601 alloy Inorganic materials 0.000 description 15
- 239000000956 alloy Substances 0.000 description 15
- 229910052786 argon Inorganic materials 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 10
- 239000007789 gas Substances 0.000 description 10
- 238000005259 measurement Methods 0.000 description 7
- 239000000523 sample Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 3
- 238000005299 abrasion Methods 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000007373 indentation Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 229910009043 WC-Co Inorganic materials 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- -1 argon ions Chemical class 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000004453 electron probe microanalysis Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000007733 ion plating Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005477 sputtering target Methods 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
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Abstract
【課題】スパッタリング法で被覆したＡｌＣｒＳｉの窒化物の層上にＴｉＳｉの窒化物の層を設けた被覆切削工具について、耐久性を向上させる。【解決手段】基材と、基材上に形成される硬質皮膜とを備える被覆切削工具。硬質皮膜は、基材の上に設けられるＡｌＣｒＳｉの窒化物の層と、ＡｌＣｒＳｉの窒化物の層上に設けられるＴｉＳｉの窒化物の層とを有する。硬質皮膜は、Ｘ線回折において面心立方格子構造を示し、Ｘ線回折により求めた２θが３７°～３８°の範囲に（１１１）面のピークを有し、（１１１）面のＸ線回折ピークの半値幅が０．５０°以上０．６０°以下である。硬質皮膜は、半金属を含む金属元素と非金属元素の合計を１００原子％とした場合、Ａｒを０．２原子％以下で含有している。【選択図】図１[Problem] To improve the durability of a coated cutting tool in which a TiSi nitride layer is provided on an AlCrSi nitride layer coated by a sputtering method. [Solution] A coated cutting tool comprising a substrate and a hard coating formed on the substrate. The hard coating comprises an AlCrSi nitride layer provided on the substrate and a TiSi nitride layer provided on the AlCrSi nitride layer. The hard coating exhibits a face-centered cubic lattice structure in X-ray diffraction, has a (111) plane peak in the range of 2θ of 37° to 38° as determined by X-ray diffraction, and has a half-width of the X-ray diffraction peak of the (111) plane of 0.50° to 0.60°. The hard coating contains 0.2 atomic % or less of Ar when the total of metal elements including metalloids and nonmetal elements is 100 atomic %. [Selected Figure] Figure 1
Description
本発明は、被覆切削工具に関する。 The present invention relates to a coated cutting tool.
ＡｌＣｒＳｉ窒化物の層上にＴｉＳｉ窒化物の層を設けた被覆切削工具は耐久性に優れており種々検討がされている。例えば、特許文献１にはアークイオンプレーティング法により、基材の表面にＴｉボンバード層を形成した後にＡｌＣｒＳｉの窒化物の層を設けてその上にＴｉＳｉの窒化物の層を設けた被覆切削工具を開示している。 Coated cutting tools in which a layer of TiSi nitride is provided on a layer of AlCrSi nitride have excellent durability and are being studied in various ways. For example, Patent Document 1 discloses a coated cutting tool in which a Ti bombarded layer is formed on the surface of a substrate by arc ion plating, and then a layer of AlCrSi nitride is provided on top of that, and a layer of TiSi nitride is provided on top of that.
近年、被覆切削工具において高出力スパッタリング法が適用され始めている。本発明者等の検討によると、スパッタリング法で被覆したＡｌＣｒＳｉの窒化物の層上にＴｉＳｉの窒化物の層を設けた被覆切削工具について、耐久性に改善の余地があることを確認した。 In recent years, high-power sputtering has begun to be used for coated cutting tools. The inventors' research has confirmed that there is room for improvement in the durability of coated cutting tools in which a TiSi nitride layer is provided on an AlCrSi nitride layer coated by sputtering.
本発明の一態様は、基材と、前記基材上に形成される硬質皮膜とを備え、前記硬質皮膜は、前記基材の上に設けられるＡｌＣｒＳｉの窒化物の層と、前記ＡｌＣｒＳｉの窒化物の層上に設けられるＴｉＳｉの窒化物の層とを有し、Ｘ線回折において面心立方格子構造を示し、前記Ｘ線回折により求めた２θが３７°～３８°の範囲に（１１１）面のピークを有し、前記（１１１）面のＸ線回折ピークの半値幅が０．５０°以上０．６０°以下であり、半金属を含む金属元素と非金属元素の合計を１００原子％とした場合、Ａｒを０．２原子％以下で含有している被覆切削工具である。 One aspect of the present invention is a coated cutting tool comprising a substrate and a hard coating formed on the substrate, the hard coating having an AlCrSi nitride layer provided on the substrate and a TiSi nitride layer provided on the AlCrSi nitride layer, exhibiting a face-centered cubic lattice structure in X-ray diffraction, having a (111) plane peak in the range of 2θ of 37° to 38° as determined by the X-ray diffraction, the half-width of the X-ray diffraction peak of the (111) plane being 0.50° or more and 0.60° or less, and containing 0.2 atomic % or less of Ar when the total of metal elements including metalloids and nonmetal elements is 100 atomic %.
本発明によれば、耐久性に優れる被覆切削工具を提供することができる。 The present invention provides a coated cutting tool with excellent durability.
本発明者等は、スパッタリング法によりＡｌＣｒＳｉの窒化物の層とＴｉＳｉの窒化物の層とを設けた被覆切削工具について、Ｘ線回折における（１１１）面のピーク強度の半値幅が一定範囲にあるときに耐久性が優れることを確認して本発明に到達した。以下、詳細に説明する。 The inventors of the present invention have confirmed that a coated cutting tool having an AlCrSi nitride layer and a TiSi nitride layer formed by a sputtering method has excellent durability when the half-width of the peak intensity of the (111) plane in X-ray diffraction is within a certain range. This will be explained in detail below.
本実施形態の被覆切削工具においては、基材は特段限定されないが、強度と靭性に優れるＷＣ－Ｃｏ基超硬合金を基材とすることが好ましい。 In the coated cutting tool of this embodiment, the substrate is not particularly limited, but it is preferable to use a WC-Co-based cemented carbide substrate, which has excellent strength and toughness.
本実施形態の被覆切削工具においては、基材の上にＡｌＣｒＳｉの窒化物の層を設ける。ＡｌＣｒＳｉの窒化物の層は耐熱性と耐摩耗性の優れる膜種であり、ＴｉＳｉの窒化物の層の下層として設けることで被覆切削工具の耐久性を高めることができる。本実施形態に係るＡｌＣｒＳｉの窒化物の層は、金属（半金属を含む。以下同様。）元素の総量に対して、Ａｌは５０原子％以上７０原子％以下が好ましい。Ｃｒは３０原子％以上４５原子％以下が好ましい。Ｓｉは１原子％以上１０原子％以下が好ましい。更には、Ｓｉは１原子％以上３原子％以下が好ましい。Ｓｉの添加量を少なくすることでｈｃｐ構造のＡｌＮが低減して好ましい。
本実施形態に係るＡｌＣｒＳｉの窒化物の層はナノインデンテーション硬度が３０ＧＰａ以上３５ＧＰａ以下、弾性率が５２０ＧＰａ以上６２０ＧＰａ以下であることが好ましい。
In the coated cutting tool of this embodiment, an AlCrSi nitride layer is provided on the substrate. The AlCrSi nitride layer is a film type with excellent heat resistance and wear resistance, and by providing it as an underlayer of the TiSi nitride layer, the durability of the coated cutting tool can be improved. In the AlCrSi nitride layer according to this embodiment, Al is preferably 50 atomic % or more and 70 atomic % or less with respect to the total amount of metal (including metalloid, the same applies below). Cr is preferably 30 atomic % or more and 45 atomic % or less. Si is preferably 1 atomic % or more and 10 atomic % or less. Furthermore, Si is preferably 1 atomic % or more and 3 atomic % or less. By reducing the amount of Si added, AlN with a hcp structure is reduced, which is preferable.
The AlCrSi nitride layer according to this embodiment preferably has a nanoindentation hardness of 30 GPa or more and 35 GPa or less, and an elastic modulus of 520 GPa or more and 620 GPa or less.
本実施形態の被覆切削工具においては、上述したＡｌＣｒＳｉの窒化物の層上にはＴｉＳｉの窒化物の層を設ける。ＴｉＳｉの窒化物は皮膜組織が微細で高い硬度を有する膜種であり、ＡｌＣｒＳｉの窒化物の上層として設けることで被覆切削工具の耐久性を高めることができる。本実施形態に係るＴｉＳｉの窒化物の層は、ナノインデンテーション硬度が４０ＧＰａ以上であることが好ましい。Ｔｉは６０原子％以上９０原子％以下が好ましい。Ｓｉは１０原子％以上４０原子％以下が好ましい。 In the coated cutting tool of this embodiment, a layer of TiSi nitride is provided on the layer of AlCrSi nitride described above. TiSi nitride is a film type with a fine film structure and high hardness, and providing it as an upper layer of AlCrSi nitride can increase the durability of the coated cutting tool. The TiSi nitride layer according to this embodiment preferably has a nanoindentation hardness of 40 GPa or more. Ti is preferably 60 atomic % or more and 90 atomic % or less. Si is preferably 10 atomic % or more and 40 atomic % or less.
本実施形態に係る硬質皮膜は、Ｘ線回折において面心立方格子構造を示し、Ｘ線回折により求めた２θが３７°～３８°の範囲に（１１１）面のピークを有する。このピークはＣｒＮに由来するピークであり、ＡｌＣｒＳｉの窒化物を評価するのに適している。
本実施形態に係る硬質皮膜は、２θが３７°～３８°にある（１１１）面のＸ線回折ピークの半値幅が０．５０°以上０．６０°以下である。これによりＡｌＣｒＳｉの窒化物の層が硬度、弾性係数および圧縮残留応力を低下させずに皮膜組織が微細になり被覆切削工具の耐久性を高めることができる。
Ｘ線回折は、市販のＸ線回折装置を用い、管電圧４５ｋＶ、管電流４０ｍＡ、Ｘ線源Ｃｕｋα（λ＝０．１５４０５ｎｍ）、２θが２０～８０度の測定条件で測定すればよい。
The hard coating according to this embodiment exhibits a face-centered cubic lattice structure in X-ray diffraction, and has a (111) peak in the range of 2θ of 37° to 38° as determined by X-ray diffraction. This peak is derived from CrN and is suitable for evaluating AlCrSi nitrides.
In the hard coating according to this embodiment, the half-width of the X-ray diffraction peak of the (111) plane at 2θ of 37° to 38° is 0.50° or more and 0.60° or less, which allows the AlCrSi nitride layer to have a fine coating structure without reducing the hardness, elastic modulus, and compressive residual stress, thereby improving the durability of the coated cutting tool.
X-ray diffraction may be measured using a commercially available X-ray diffraction device under measurement conditions of a tube voltage of 45 kV, a tube current of 40 mA, an X-ray source Cukα (λ=0.15405 nm), and 2θ of 20 to 80 degrees.
本実施形態に係るＡｌＣｒＳｉの窒化物の層は、制限視野回折パターンの輝度から求められる強度プロファイルにおいてｈｃｐ構造のＡｌＮに起因するピークを有しないことが好ましい。ミクロレベルでｈｃｐ構造のＡｌＮが少ないことで被覆切削工具の耐久性を高めることができる。本実施形態においては、制限視野回折パターンの輝度から求められる強度プロファイルはバックグラウンドを除去して評価する。 The AlCrSi nitride layer according to this embodiment preferably does not have a peak due to AlN with a hcp structure in the intensity profile determined from the brightness of the selected area diffraction pattern. Having less AlN with a hcp structure at the micro level can increase the durability of the coated cutting tool. In this embodiment, the intensity profile determined from the brightness of the selected area diffraction pattern is evaluated after removing the background.
本実施形態に係る硬質皮膜については、半金属を含む金属元素と非金属元素の総量を１００原子％とした場合、アルゴン（Ａｒ）を０．２原子％以下で含有する。
スパッタリング法では、アルゴンイオンを用いてターゲット成分をスパッタリングして
硬質皮膜を被覆するため、硬質皮膜にアルゴンを含有させやすい。硬質皮膜の結晶粒径が微粒化すると硬度が高まる一方、結晶粒界が多くなり、硬質皮膜に含有されるアルゴンが結晶粒界に濃化する。硬質皮膜のアルゴン含有比率が大きすぎる場合には、硬質皮膜の靭性が低下し、十分な工具性能が発揮され難い。そのため、本実施形態では硬質皮膜の結晶粒界に濃化するアルゴンを低減させるよう、半金属を含む金属元素と非金属元素の総量を１００原子％とした場合、アルゴンを０．２原子％以下で含有させる。本実施形態においては、アルゴン（Ａｒ）の含有比率の下限を特段限定するものではない。本実施形態に係る硬質皮膜は、スパッタリング法で被覆するため、アルゴン（Ａｒ）を０．０１原子％以上で含有し得る。
The hard coating according to this embodiment contains argon (Ar) at 0.2 atomic % or less when the total amount of metal elements including metalloids and nonmetal elements is taken as 100 atomic %.
In the sputtering method, the target components are sputtered using argon ions to coat the hard film, so that it is easy to make the hard film contain argon. When the grain size of the hard film is finer, the hardness increases, while the grain boundaries increase, and the argon contained in the hard film is concentrated at the grain boundaries. If the argon content ratio of the hard film is too high, the toughness of the hard film decreases, and it is difficult to exhibit sufficient tool performance. Therefore, in this embodiment, in order to reduce the argon concentrated at the grain boundaries of the hard film, argon is contained at 0.2 atomic % or less when the total amount of metal elements including metalloids and nonmetal elements is 100 atomic %. In this embodiment, the lower limit of the content ratio of argon (Ar) is not particularly limited. Since the hard film according to this embodiment is coated by the sputtering method, it may contain argon (Ar) at 0.01 atomic % or more.
本実施形態に係る硬質皮膜については、ＡｌＣｒＳｉの窒化物の層の膜厚をｔ１、ＴｉＳｉの窒化物の層の膜厚をｔ２とした場合、ｔ１／ｔ２が０．７以上１．３以下であることが好ましい。ＡｌＣｒＳｉの窒化物の層とＴｉＳｉの窒化物の層の膜厚が同程度であることで被覆切削工具の耐久性が優れるものとなる。ｔ１は０．５μｍ以上３μｍ以下が好ましい。ｔ２は０．５μｍ以上３μｍ以下が好ましい。 For the hard coating according to this embodiment, when the thickness of the AlCrSi nitride layer is t1 and the thickness of the TiSi nitride layer is t2, it is preferable that t1/t2 is 0.7 or more and 1.3 or less. By making the thickness of the AlCrSi nitride layer and the TiSi nitride layer approximately the same, the durability of the coated cutting tool becomes excellent. t1 is preferably 0.5 μm or more and 3 μm or less. t2 is preferably 0.5 μm or more and 3 μm or less.
本実施形態の被覆切削工具は、基材とＡｌＣｒＳｉ窒化物の層との間には中間皮膜を設けても良い。ＡｌＣｒＳｉの窒化物の層とＴｉＳｉの窒化物の層との間には、ＡｌＣｒＳｉの窒化物の層とＴｉＳｉの窒化物の層とが交互に積層した積層皮膜を設けてもよい。
積層皮膜の合計膜厚は、積層皮膜の下側に位置するＡｌＣｒＳｉの窒化物の層の膜厚よりも小さいことが好ましい。積層皮膜の合計膜厚は、積層皮膜の上側に位置するＴｉＳｉの窒化物の層の膜厚よりも小さいことが好ましい。積層皮膜の構成層の膜厚は、１ｎｍ以上１０ｎｍ以下の範囲であることが好ましい。ナノレベルで交互に積層する積層皮膜は互いの層の組成が混ざり合う。そのため、ナノレベルで交互に積層するＡｌＣｒＳｉの窒化物の層とＴｉＳｉの窒化物の層について、ＡｌＣｒＳｉの窒化物の層はＴｉを含有し、積層皮膜のＴｉＳｉの窒化物の層はＡｌとＣｒを含有する。積層皮膜の合計膜厚をｔ３とした場合、ｔ３／（ｔ１＋ｔ２＋ｔ３）が０．０５以上０．３以下であることが好ましい。更には、ｔ３／（ｔ１＋ｔ２＋ｔ３）が０．０７以上０．２以下であることが好ましい。上層のＴｉＳｉの窒化物の層上に、さらに別の硬質皮膜を設けてもよい。
In the coated cutting tool of this embodiment, an intermediate coating may be provided between the substrate and the AlCrSi nitride layer, and a laminate coating in which layers of AlCrSi nitride and layers of TiSi nitride are alternately laminated may be provided between the AlCrSi nitride layer and the TiSi nitride layer.
The total thickness of the laminated film is preferably smaller than the thickness of the AlCrSi nitride layer located below the laminated film. The total thickness of the laminated film is preferably smaller than the thickness of the TiSi nitride layer located above the laminated film. The thickness of the constituent layers of the laminated film is preferably in the range of 1 nm to 10 nm. The compositions of the layers of the laminated film alternately laminated at the nano level are mixed together. Therefore, for the AlCrSi nitride layer and the TiSi nitride layer alternately laminated at the nano level, the AlCrSi nitride layer contains Ti, and the TiSi nitride layer of the laminated film contains Al and Cr. When the total thickness of the laminated film is t3, it is preferable that t3/(t1+t2+t3) is 0.05 to 0.3. Furthermore, it is preferable that t3/(t1+t2+t3) is 0.07 to 0.2. Another hard film may be provided on the upper TiSi nitride layer.
本実施形態に係る硬質皮膜はスパッタリング法で被覆されるスパッタ皮膜である。スパッタリング法の中でも、ターゲットに順次電力を印加するスパッタリング法を適用して、電力が印加されるターゲットが切り替わる際に、電力の印加が終了するターゲットと電力の印加を開始するターゲットの両方のターゲットに同時に電力が印加されている時間を設けるスパッタリング法を適用することが好ましい。
電力パルスの最大電力密度は、０．５ｋＷ／ｃｍ２以上とすることが好ましい。電力の印加が終了する合金ターゲットと電力の印加を開始する合金ターゲットの両方の合金ターゲットに同時に電力が印加されている時間は５マイクロ秒以上２０マイクロ秒以下とすることが好ましい。ターゲット成分のイオン化率を高めるために、ＡｌＣｒＳｉ系合金ターゲット３個以上とＴｉＳｉ系合金ターゲット３個以上用いることが好ましい。
スパッタリング装置の炉内温度を４３０℃以上として予備放電を実施し、炉内に導入する窒素ガスの流量を３５０ｓｃｃｍ以上、アルゴンガスの流量を３００ｓｃｃｍ以上４５０ｓｃｃｍ以下とすることが好ましい。炉内圧力は０．６Ｐａ～０．８Ｐａとすることが好ましい。基体となる切削工具に印加する負のバイアス電圧は、－８０Ｖ～－４０Ｖの範囲に制御することが好ましい。硬質皮膜は炉内温度を５００℃以上５５０℃以下で被覆することが好ましい。
The hard coating according to the present embodiment is a sputtered coating formed by a sputtering method. Among the sputtering methods, it is preferable to use a sputtering method in which power is sequentially applied to targets, and when the target to which power is applied is switched, a time is provided during which power is simultaneously applied to both the target to which power application ends and the target to which power application starts.
The maximum power density of the power pulse is preferably 0.5 kW/ cm2 or more. The time during which power is simultaneously applied to both the alloy target to which power application ends and the alloy target to which power application starts is preferably 5 microseconds or more and 20 microseconds or less. In order to increase the ionization rate of the target components, it is preferable to use three or more AlCrSi-based alloy targets and three or more TiSi-based alloy targets.
It is preferable to carry out preliminary discharge with the temperature inside the sputtering apparatus set to 430°C or higher, and to set the flow rate of nitrogen gas introduced into the furnace to 350 sccm or higher, and the flow rate of argon gas to 300 sccm or higher and 450 sccm or lower. The pressure inside the furnace is preferably set to 0.6 Pa to 0.8 Pa. The negative bias voltage applied to the cutting tool as the substrate is preferably controlled in the range of -80 V to -40 V. The hard coating is preferably applied at a furnace temperature of 500°C to 550°C.
本実施形態の硬質皮膜は、スパッタリングターゲットに含まれる不可避不純物を含む場合がある。硬質皮膜中の不可避不純物は、硬質皮膜の性能に影響を与えない範囲であれば含有を許容される。本実施形態の硬質皮膜では、半金属を含む金属元素および窒素以外の不純物の含有量は、ＥＰＭＡ（電子線マイクロアナライザー）による定量分析で、各元素について１原子％以下であることが好ましい。 The hard coating of this embodiment may contain unavoidable impurities contained in the sputtering target. The unavoidable impurities in the hard coating are permitted to be present within a range that does not affect the performance of the hard coating. In the hard coating of this embodiment, the content of impurities other than metal elements, including metalloids, and nitrogen is preferably 1 atomic % or less for each element as determined by quantitative analysis using an EPMA (electron probe microanalyzer).
以下、実施例および比較例により本発明をさらに具体的に説明するが、本発明は以下の実施例に限定されるものではない。 The present invention will be explained in more detail below with reference to examples and comparative examples, but the present invention is not limited to the following examples.
＜工具＞
工具として、組成がＷＣ（ｂａｌ．）－Ｃｏ（８．０質量％）－Ｃｒ（０．５質量％）－Ｔａ（０．３質量％）、ＷＣ平均粒度０．５μｍ、硬度９３．６ＨＲＡ（ロックウェル硬さ、ＪＩＳ Ｇ ０２０２に準じて測定した値）からなる超硬合金製の２枚刃ボールエンドミル（工具径０．８ｍｍ、株式会社ＭＯＬＤＩＮＯ製）を準備した。
<Tools>
As a tool, a two-blade ball end mill (tool diameter 0.8 mm, manufactured by MOLDINO Co., Ltd.) made of cemented carbide having a composition of WC (bal.)-Co (8.0 mass%)-Cr (0.5 mass%)-Ta (0.3 mass%), an average WC grain size of 0.5 μm, and a hardness of 93.6 HRA (Rockwell hardness, a value measured in accordance with JIS G 0202) was prepared.
スパッタ蒸発源を１２機搭載できるスパッタリング装置を使用した。これらの蒸着源のうち、ＡｌＣｒＳｉ系合金ターゲット（Ａｌ５８％Ｃｒ４０％Ｓｉ２％ 数字は原子比率、以下同様。）６個およびＴｉＳｉ系合金ターゲット（Ｔｉ８０％Ｓｉ２０％）６個を蒸着源として装置内に設置した。なお、寸法が直径１６ｃｍ、厚み１２ｍｍのターゲットを用いた。
工具をスパッタリング装置内のサンプルホルダーに固定し、工具にバイアス電源を接続した。なお、バイアス電源は、ターゲットとは独立して工具に負のバイアス電圧を印加する構造となっている。工具は、毎分３回転で自転し、かつ、固定治具とサンプルホルダーを介して公転する。工具とターゲット表面との間の最近接距離を１００ｍｍとした。
導入ガスは、ＡｒおよびＮ２を用い、スパッタリング装置に設けられたガス供給ポートから導入した。
A sputtering device capable of mounting 12 sputter evaporation sources was used. Among these evaporation sources, six AlCrSi alloy targets (Al58%Cr40%Si2%; numbers indicate atomic ratios, the same applies below) and six TiSi alloy targets (Ti80%Si20%) were installed in the device as evaporation sources. The targets used had a diameter of 16 cm and a thickness of 12 mm.
The tool was fixed to a sample holder in a sputtering apparatus, and a bias power supply was connected to the tool. The bias power supply was structured to apply a negative bias voltage to the tool independently of the target. The tool rotated at three revolutions per minute and revolved around the fixture and the sample holder. The closest distance between the tool and the target surface was set to 100 mm.
The gases used were Ar and N2 , and were introduced from a gas supply port provided in the sputtering device.
＜ボンバード処理＞
まず、工具に硬質皮膜を被覆する前に、以下の手順で工具にボンバード処理を行った。スパッタリング装置内のヒーターにより炉内温度が４３０℃になった状態で３０分間の加熱を行った。その後、スパッタリング装置の炉内を真空排気し、炉内圧力を５．０×１０－３Ｐａ以下とした。そして、Ａｒガスをスパッタリング装置の炉内に導入し、炉内圧力を０．８Ｐａに調整した。そして、工具に－２００Ｖの直流バイアス電圧を印加して、Ａｒイオンによる工具のクリーニング（ボンバード処理）を実施した。
<Bombardment Processing>
First, before the tool was coated with a hard coating, the tool was bombarded in the following manner. Heating was performed for 30 minutes with the furnace temperature at 430° C. by a heater in the sputtering device. Thereafter, the furnace of the sputtering device was evacuated to a vacuum and the furnace pressure was set to 5.0×10 −3 Pa or less. Then, Ar gas was introduced into the furnace of the sputtering device, and the furnace pressure was adjusted to 0.8 Pa. Then, a DC bias voltage of −200 V was applied to the tool, and cleaning (bombardment) of the tool with Ar ions was performed.
本実施例１について、ボンバード処理後、炉内温度を５１０℃に保持したまま、スパッタリング装置の炉内にＡｒガスを４００ｓｃｃｍで導入し、その後、Ｎ２ガスを４７０ｓｃｃｍで導入して炉内圧力を０．７２Ｐａとした。次いで、工具に－５０Ｖの直流バイアス電圧を印加して、ＡｌＣｒＳｉ系合金ターゲットに印加に１．５ｋＷ／ｃｍ２の最大電力密度を印加し、電力の１周期当りの放電時間を３．６ミリ秒、ＡｌＣｒＳｉ系合金ターゲットに同時に電力が印加されている時間を１０マイクロ秒として膜厚が約０．６μｍのＡｌＣｒＳｉの窒化物の層を被覆した。 In this embodiment 1, after the bombardment process, while the temperature inside the furnace was kept at 510° C., Ar gas was introduced into the furnace of the sputtering device at 400 sccm, and then N 2 gas was introduced at 470 sccm to set the pressure inside the furnace to 0.72 Pa. Next, a DC bias voltage of −50 V was applied to the tool, and a maximum power density of 1.5 kW/cm 2 was applied to the AlCrSi alloy target, with the discharge time per power cycle being 3.6 milliseconds and the time during which power was simultaneously applied to the AlCrSi alloy target being 10 microseconds, to coat a layer of AlCrSi nitride having a film thickness of about 0.6 μm.
次いで、炉内温度を５１０℃に保持したまま、スパッタリング装置の炉内にＡｒガスを４００ｓｃｃｍで導入し、その後、Ｎ２ガスを４１０ｓｃｃｍで導入して炉内圧力を０．７Ｐａとした。次いで、工具に－５０Ｖの直流バイアス電圧を印加して、ＡｌＣｒＳｉ系合金ターゲットに１．５ｋＷ／ｃｍ２の最大電力密度を印加して、電力の１周期当りの放電時間を３．６ミリ秒、ＡｌＣｒＳｉ系合金ターゲットに同時に電力が印加されている時間を１０マイクロ秒とした。また、ＴｉＳｉ系合金ターゲットに１．５ｋＷ／ｃｍ２の最大電力密度を印加して、電力の１周期当りの放電時間を３．６ミリ秒、ＴｉＳｉ系合金ターゲットに同時に電力が印加されている時間を１０マイクロ秒とした。そして、それぞれの合金ターゲットに連続的に電力を印加して、個々の層の膜厚が約４ｎｍで総膜厚が約０．１μｍの積層皮膜を被覆した。この積層皮膜は、ＡｌＣｒＳｉの窒化物の層とＴｉＳｉの窒化物の層が交互に積層された硬質皮膜である。積層皮膜において、ＡｌＣｒＳｉの窒化物の層はＴｉを含有し、ＴｉＳｉの窒化物の層はＡｌとＣｒを含有している。 Next, while the furnace temperature was maintained at 510°C, Ar gas was introduced into the furnace of the sputtering device at 400 sccm, and then N2 gas was introduced at 410 sccm to set the furnace pressure to 0.7 Pa. Next, a DC bias voltage of -50V was applied to the tool, and a maximum power density of 1.5 kW/ cm2 was applied to the AlCrSi alloy target, with the discharge time per power cycle being 3.6 milliseconds and the time during which power was simultaneously applied to the AlCrSi alloy target being 10 microseconds. Also, a maximum power density of 1.5 kW/ cm2 was applied to the TiSi alloy target, with the discharge time per power cycle being 3.6 milliseconds and the time during which power was simultaneously applied to the TiSi alloy target being 10 microseconds. Then, power was applied continuously to each alloy target to coat a laminated film with an individual layer thickness of about 4 nm and a total thickness of about 0.1 μm. This laminate coating is a hard coating in which layers of AlCrSi nitride and layers of TiSi nitride are alternately laminated, in which the layers of AlCrSi nitride contain Ti, and the layers of TiSi nitride contain Al and Cr.
次いで、炉内温度を５１０℃に保持したまま、スパッタリング装置の炉内にＡｒガスを４００ｓｃｃｍで導入し、その後、Ｎ２ガスを２７０ｓｃｃｍで導入して炉内圧力を０．５４Ｐａとした。工具に－５０Ｖの直流バイアス電圧を印加して、ＴｉＳｉ系合金ターゲットに１．５ｋＷ／ｃｍ２の最大電力密度を印加して、印加電力の１周期当りの放電時間を３．６ミリ秒、ＴｉＳｉ系合金ターゲットに同時に電力が印加されている時間を１０マイクロ秒として膜厚が約０．４μｍのＴｉＳｉの窒化物の層を被覆した。 Next, while the furnace temperature was kept at 510° C., Ar gas was introduced into the furnace of the sputtering device at 400 sccm, and then N 2 gas was introduced at 270 sccm to set the furnace pressure to 0.54 Pa. A DC bias voltage of −50 V was applied to the tool, and a maximum power density of 1.5 kW/cm 2 was applied to the TiSi-based alloy target, with the discharge time per cycle of the applied power being 3.6 milliseconds and the time during which power was simultaneously applied to the TiSi-based alloy target being 10 microseconds, to coat a layer of TiSi nitride with a film thickness of about 0.4 μm.
本実施例２は硬質皮膜の各層の被覆時に、炉内温度を５４０℃とした以外は本実施例１と同じとした。
比較例１は硬質皮膜の各層の被覆時に、炉内温度を４３０℃とした以外は本実施例１と同じとした。
比較例２は硬質皮膜の各層の被覆時に、炉内温度を４５０℃とした以外は本実施例１と同じとした。
比較例３は硬質皮膜の各層の被覆時に、炉内温度を４８０℃とした以外は本実施例１と同じとした。
比較例４は硬質皮膜の各層の被覆時に、炉内温度を５７０℃とした以外は本実施例１と同じとした。
Example 2 was the same as Example 1, except that the temperature inside the furnace was 540° C. when each layer of the hard coating was applied.
Comparative Example 1 was the same as Example 1, except that the temperature inside the furnace was 430° C. when each layer of the hard coating was applied.
Comparative Example 2 was the same as Example 1, except that the temperature inside the furnace was 450° C. when each layer of the hard coating was applied.
Comparative Example 3 was the same as Example 1, except that the temperature inside the furnace was 480° C. when each layer of the hard coating was applied.
Comparative Example 4 was the same as Example 1, except that the temperature inside the furnace was 570° C. when each layer of the hard coating was applied.
硬質皮膜の皮膜組成は、電子プローブマイクロアナライザー装置（株式会社日本電子製 ＪＸＡ－８５００Ｆ）に付属する波長分散型電子プローブ微小分析（ＷＤＳ－ＥＰＭＡ）で測定した。物性評価用のボールエンドミルを鏡面加工して、加速電圧１０ｋＶ、照射電流５×１０－８Ａ、取り込み時間１０秒とし、分析領域が直径１μｍの範囲を５点測定してその平均値からＡｒの含有比率を求めた。 The composition of the hard coating was measured by a wavelength dispersive electron probe microanalysis (WDS-EPMA) attached to an electron probe microanalyzer (JXA-8500F, manufactured by JEOL Ltd.) A ball end mill for evaluating physical properties was mirror-finished, and measurements were taken at five points over an analysis area of 1 μm in diameter at an acceleration voltage of 10 kV, a probe current of 5×10 −8 A, and a capture time of 10 seconds, and the Ar content was calculated from the average value.
Ｘ線回折装置（株式会社ＰａＮａｌｙｔｉｃａｌ製 ＥＭＰＹＲＥＡ）を用い、管電圧４５ｋＶ、管電流４０ｍＡ、Ｘ線源Ｃｕｋα（λ＝０．１５４０５ｎｍ）、２θが２０～８０度の測定条件で結晶構造の確認及び半値幅の測定を行った。 The crystal structure was confirmed and the half-width was measured using an X-ray diffraction device (EMPYREA manufactured by PaNalytical Co., Ltd.) under the following measurement conditions: tube voltage 45 kV, tube current 40 mA, X-ray source Cukα (λ = 0.15405 nm), 2θ 20 to 80 degrees.
ＡｌＣｒＳｉの窒化物の層についてナノインデンテーションテスター（株式会社エリオニクス社製ＥＮＴ－２１００）を用いて硬度と弾性係数を分析した。分析は、皮膜の最表面に対し試験片を５度傾けた皮膜断面を鏡面研磨後、皮膜の研磨面内で最大押し込み深さが膜厚の略１／１０未満となる領域を選定した。押し込み荷重９．８０７ｍＮの測定条件で１５点測定し、値の大きい側の５点と値の小さい側の５点を除いた５点の平均値から求めた。 The hardness and elastic modulus of the AlCrSi nitride layer were analyzed using a nanoindentation tester (ENT-2100, manufactured by Elionix Co., Ltd.). For the analysis, the cross section of the film was mirror-polished by tilting a test piece 5 degrees relative to the outermost surface of the film, and then an area within the polished surface of the film where the maximum indentation depth was approximately 1/10 of the film thickness was selected. 15 points were measured under measurement conditions of an indentation load of 9.807 mN, and the hardness and elastic modulus were calculated from the average value of the five points excluding the five points with the largest value and the five points with the smallest value.
硬質皮膜の残留圧縮応力は、粗さ測定器（東京精密製表面粗さ測定器ＤＸ－２３）を用い、測定長さ２２ｍｍ、測定速度１．５ｍｍ／ｓの測定条件で試料のたわみ量を測定し、次式を用いて算出した。なお、Ｅｓ値は基材のヤング率、Ｄ値は試験片の厚み、δ値は被覆前後で生じる試験片のたわみ量、Ｌ値は被覆によってたわみが生じた試験片の長さ方向端面から、最大たわみ部までの長さ、ｖｓ値は試験片に使用した基材のポアソン比、およびｄは試験片表面に被覆した硬質皮膜の膜厚である。 The residual compressive stress of the hard coating was calculated using the following formula after measuring the amount of deflection of the sample using a roughness tester (Tokyo Seimitsu Surface Roughness Tester DX-23) under measurement conditions of a measurement length of 22 mm and a measurement speed of 1.5 mm/s. The Es value is the Young's modulus of the substrate, the D value is the thickness of the test piece, the δ value is the amount of deflection of the test piece before and after coating, the L value is the length from the longitudinal end face of the test piece where deflection occurred due to coating to the maximum deflection point, the vs value is the Poisson's ratio of the substrate used for the test piece, and d is the film thickness of the hard coating coated on the surface of the test piece.
（式） σ＝Ｅｓ＊Ｄ２＊δ／３＊Ｉ２＊（１－νｓ）＊ｄ (Formula) σ=Es* D2 *δ/3* I2 *(1-νs)*d
（条件）乾式加工
工具：２枚刃超硬ボールエンドミル
型番：ＥＰＤＢＥ２０１０－６、ボール半径０．５ｍｍ
切削方法：底面切削
被削材：ＳＴＡＶＡＸ（５２ＨＲＣ）（ボーラー・ウッデホルム株式会社製）
切り込み：軸方向、０．０３ｍｍ、径方向、０．０３ｍｍ
切削速度：６７．８ｍ／ｍｉｎ
一刃送り量：０．０１３５ｍｍ／刃
切削距離：１５ｍ
評価方法：切削加工後、走査型電子顕微鏡を用いて倍率１０００倍で観察し、工具逃げ面において工具と被削材が擦過した幅を測定し、そのうちの擦過幅が最も大きかった部分を逃げ面最大摩耗幅とした。
(Conditions) Dry machining Tool: 2-blade carbide ball end mill Model: EPDBE2010-6, ball radius 0.5 mm
Cutting method: Bottom cutting Workpiece: STAVAX (52HRC) (manufactured by BOHER-Uddeholm Co., Ltd.)
Cut: Axial direction, 0.03 mm, Radial direction, 0.03 mm
Cutting speed: 67.8 m/min
Feed per blade: 0.0135 mm/blade Cutting distance: 15 m
Evaluation method: After cutting, the cutting surfaces were observed at a magnification of 1000 times using a scanning electron microscope, and the width of the abrasion between the tool and the workpiece on the tool flank was measured. The part with the largest abrasion width was recorded as the maximum abrasion width on the flank.
何れの硬質皮膜も結晶構造は面心立方格子構造であり、アルゴンを０．０１～０．０３原子％の範囲で含有していた。
組織観察写真の代表例として図１に本実施例１、図２に比較例１の破断面観察写真を示す。被覆温度が高い本実施例１、２と比較例４はＡｌＣｒＳｉの窒化物の層が微細化していた。一方、上層のＴｉＳｉの窒化物の層は被覆温度による大きな組織変化は確認されなかった。
Ｘ線回折の代表例として本実施例１のＸ線回折結果を図３に示す。本実施例１、２の（１１１）面の半値幅は０．５６°～０．５７°であり、他に比べて値が小さくなった。比較例４のＡｌＣｒＳｉの窒化物の層は微細化していたが、被覆温度が高すぎるため（１１１）面の半値幅の値は大きくなり、本実施例に比べて硬度、弾性係数及び残留応力が低くなっていた。
本実施例１、２は比較例に比べて皮膜特性および被覆切削工具の耐久性が優れた。本実施例１、２は硬質皮膜の（１１１）面の半値幅が０．５６°～０．５７°であることで、皮膜組織が微細化しつつも、硬度、弾性率および圧縮残留応力が高く、被覆切削工具の耐久性に優れたと推定される。
All of the hard coatings had a face-centered cubic lattice crystal structure and contained argon in the range of 0.01 to 0.03 atomic %.
As representative examples of microstructural observation photographs, Fig. 1 shows the fracture surface observation photographs of Example 1, and Fig. 2 shows the fracture surface observation photographs of Comparative Example 1. In Examples 1 and 2 and Comparative Example 4, which were coated at high temperatures, the AlCrSi nitride layer was refined. On the other hand, no significant microstructural change due to the coating temperature was confirmed in the upper TiSi nitride layer.
As a representative example of X-ray diffraction, the X-ray diffraction results of this Example 1 are shown in Figure 3. The half-width of the (111) plane of this Example 1 and 2 was 0.56° to 0.57°, which was smaller than the other values. The AlCrSi nitride layer of Comparative Example 4 was finer, but the half-width of the (111) plane was larger because the coating temperature was too high, and the hardness, elastic modulus, and residual stress were lower than those of this Example.
The coating properties and the durability of the coated cutting tool were superior to those of the comparative example in Examples 1 and 2. It is presumed that the half-width of the (111) plane of the hard coating in Examples 1 and 2 was 0.56° to 0.57°, and therefore the coating structure was fine, while the hardness, elastic modulus, and compressive residual stress were high, and the durability of the coated cutting tool was superior.
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