JP6789503B2 - Hard film film formation method - Google Patents
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本発明は、ドリル等の切削工具やブローチ等の歯切工具の表面に被覆される硬質皮膜、当該硬質皮膜が被覆された硬質皮膜被覆工具および当該皮膜を工具の表面に成膜する硬質皮膜の成膜方法に関する。 The present invention relates to a hard film coated on the surface of a cutting tool such as a drill or a gear cutting tool such as a broach, a hard film-coated tool coated with the hard film, and a hard film forming the film on the surface of the tool. Regarding the film forming method.
これまでドリル等の切削工具やブローチをはじめとする歯切工具の表面には、切刃の耐摩耗性を向上させるために、種々の硬質皮膜が被覆された状態で供されてきた。中でも、ＡｌとＣｒとを含有する、いわゆるＡｌＣｒ系の硬質皮膜は工具表面への優れた密着性と長寿命を確保できる観点から様々な工具表面を被覆する硬質皮膜として多用されてきた。 Until now, the surface of cutting tools such as drills and gear cutting tools such as brooches has been provided with various hard films coated in order to improve the wear resistance of the cutting edge. Among them, a so-called AlCr-based hard film containing Al and Cr has been widely used as a hard film for covering various tool surfaces from the viewpoint of ensuring excellent adhesion to the tool surface and long life.
例えば、特許文献１では、従来のＴｉＡｌＮ硬質皮膜よりも耐磨耗性に優れた硬質皮膜としてＴｉａＡｌｂＣｒｃ（Ｃ１−ｄＮｄ）からなる硬質皮膜（０．５５≦ｂ≦０．７６５、０．０６≦ｃ）は、近年の工具の高速化および高能率化に適合させるための成膜方法が開示されている。具体的には、成膜装置を用いた成膜時において基板に対して印加するバイアス電圧を−５０Ｖ〜−３００Ｖの範囲としたり、または基板の温度を３００℃〜８００℃の範囲として硬質皮膜を成膜する方法が説明されている。 For example, in Patent Document 1, a hard film (0.55 ≦ b ≦ 0) made of Ti a Al b Cr c (C 1-d N d ) as a hard film having superior wear resistance to the conventional TiAlN hard film. .765, 0.06 ≦ c) discloses a film forming method for adapting to the recent high speed and high efficiency of tools. Specifically, the bias voltage applied to the substrate during film formation using a film forming apparatus is set in the range of -50V to -300V, or the temperature of the substrate is set in the range of 300 ° C to 800 ° C to form a hard film. The method of forming a film is described.
しかし、特許文献１に開示されているＴｉＡｌＣｒＮ硬質皮膜はＡｌの比率が高い場合、具体的にはＡｌの比率が７５％以上では硬質皮膜の結晶構造が立方晶から六方晶に構造変化する。結晶構造が六方晶に構造変化すると、硬質皮膜の硬さが極端に失われて、硬質皮膜の耐磨耗性が著しく低下するという問題があった。 However, when the TiAlCrN hard film disclosed in Patent Document 1 has a high ratio of Al, specifically, when the ratio of Al is 75% or more, the crystal structure of the hard film changes from cubic to hexagonal. When the crystal structure is changed to hexagonal, there is a problem that the hardness of the hard film is extremely lost and the abrasion resistance of the hard film is remarkably lowered.
そこで、本発明においてはＡｌの比率が７５％以上のＡｌとＣｒとの窒化物皮膜であっても、結晶構造を立方晶とすることで硬質皮膜の硬度を維持しつつ、硬質皮膜の耐磨耗性が向上する硬質皮膜、当該硬質皮膜を被覆した工具および当該硬質皮膜の成膜方法を提供することを課題とする。 Therefore, in the present invention, even in the case of a nitride film of Al and Cr having an Al ratio of 75% or more, the hardness of the hard film is maintained by making the crystal structure cubic, and the polishing resistance of the hard film is maintained. It is an object of the present invention to provide a hard film having improved wear resistance, a tool coated with the hard film, and a method for forming the hard film.
前述した課題を解決するために、本発明の硬質皮膜の成膜方法は、Ａｌ１−ｙＣｒｙ（０．０５≦ｙ≦０．２０）から成るターゲットを内部に備えるカソードアーク方式イオンプレーティング装置を用いた硬質皮膜の成膜方法において、カソードアーク方式イオンプレーティング装置内に設置する基板に対して印加するバイアス電圧を−１００Ｖ〜−１７０Ｖの範囲とし、基板の温度を３３０℃〜３７０℃の範囲として硬質皮膜を成膜する硬質皮膜の成膜方法とした。 To solve the problems described above, the film formation method of the hard film of the present invention, Al 1-y Cr y cathodic arc method ion plating comprising a target composed of (0.05 ≦ y ≦ 0.20) in the interior In the method of forming a hard film using an apparatus, the bias voltage applied to the substrate installed in the cathode arc ion plating apparatus is in the range of -100V to -170V, and the temperature of the substrate is set to 330 ° C. to 370 ° C. As the range of, the method of forming a hard film was used.
また、本発明の硬質皮膜は、Ａｌ１−ｘＣｒｘＮ（０．０５≦ｘ≦０．２５：ｘはＣｒの原子比率を示す。）から成る組成の硬質皮膜であって、硬質皮膜の表面をＸ線回折（２θ）した際における３０°≦２θ≦９０°の測定範囲において、Ｃｕ―Ｋα線の最も高いピークが２θ＝３７．８°±１°の範囲に存在し、かつピークの半値幅が１°未満である硬質皮膜とした。前述の硬質皮膜は、Ｃｒの一部を、０．０５以下のＴｉ、Ｖ、Ｚｒ、もしくはＮｂで置き換えた組成とすることもできる。また、硬質皮膜の厚さを０．１μｍ〜２０μｍの範囲とすることもできる。 Further, the hard film of the present invention is a hard film having a composition composed of Al 1-x Cr x N (0.05 ≦ x ≦ 0.25: x indicates the atomic ratio of Cr), and is a hard film. In the measurement range of 30 ° ≤ 2θ ≤ 90 ° when the surface is X-ray diffracted (2θ), the highest peak of Cu—Kα ray exists in the range of 2θ = 37.8 ° ± 1 °, and the peak A hard film having a half-value width of less than 1 ° was used. The above-mentioned hard film may have a composition in which a part of Cr is replaced with Ti, V, Zr, or Nb of 0.05 or less. Further, the thickness of the hard film can be in the range of 0.1 μm to 20 μm.
本発明の硬質皮膜被覆工具は、前述の硬質皮膜が超硬合金製または高速度工具鋼製の工具の表面に被覆されている硬質皮膜被覆工具とする。 The hard film coating tool of the present invention is a hard film coating tool in which the above-mentioned hard film is coated on the surface of a tool made of cemented carbide or high-speed steel.
本発明の硬質皮膜の成膜方法により、成膜された硬質皮膜の結晶構造を立方晶とすることができる。そのため、硬質皮膜の硬度を維持しつつ、硬質皮膜の耐磨耗性を向上することができるという効果を奏する。 By the method for forming a hard film of the present invention, the crystal structure of the formed hard film can be made into a cubic crystal. Therefore, it is possible to improve the abrasion resistance of the hard film while maintaining the hardness of the hard film.
次に、本発明の硬質皮膜の成膜方法に関する実施形態の一例について説明する。まず、本発明の成膜方法に用いる成膜装置は、内部にターゲットが設置されており、当該ターゲット表面にアークを発生することで、当該ターゲットを構成する金属原子のイオンを発生させることでバイアス電圧が印加された基板表面に成膜を行うアークイオンプレーティング装置とする。 Next, an example of an embodiment relating to the method for forming a hard film of the present invention will be described. First, the film forming apparatus used in the film forming method of the present invention has a target installed inside, and by generating an arc on the surface of the target, it is biased by generating ions of metal atoms constituting the target. An arc ion plating apparatus that forms a film on the surface of a substrate to which a voltage is applied.
また、当該ターゲットはＡｌ１−ｙＣｒｙ（ｙはＣｒの原子比率を示す、０．０５≦ｙ≦０．２０）から成るターゲットとする。そのような成膜装置内に基板を設置して後、当該基板に対してアルゴンガス等の不活性ガスによるイオンボンバード（表面清浄）を行う。その後、当該基板に対してバイアス電圧を−１００Ｖ〜−１７０Ｖの範囲で印加する。また、基板の温度は３３０℃〜３７０℃の範囲とする。本発明の成膜方法において、基板に基板に対するバイアス電圧および基板の温度を限定した理由は、以下の通りである。 Further, the target is a target composed of Al 1-y Cr y (y indicates the atomic ratio of Cr, 0.05 ≦ y ≦ 0.20). After the substrate is installed in such a film forming apparatus, ion bombarding (surface cleaning) is performed on the substrate with an inert gas such as argon gas. Then, a bias voltage is applied to the substrate in the range of −100V to −170V. The temperature of the substrate is in the range of 330 ° C. to 370 ° C. The reason for limiting the bias voltage with respect to the substrate and the temperature of the substrate to the substrate in the film forming method of the present invention is as follows.
まず、硬質皮膜の結晶構造に関して、立方晶の構造を得るためには局所的な高圧状態を作り出す必要があると本発明者は考えた。すなわち、成膜対象である基板への成膜物質のエネルギーを比較的に高くする必要があると考えた。そのエネルギーを高める方法として、基板のバイアス電圧を絶対値が大きい負の電圧にする方法が最も簡便であると考えた。基板の電圧が所定値以上（絶対値が小さい）になると、成膜時のエネルギーが不足するので結晶構造は六方晶となりやすい。また、所定値以下（絶対値が大きい）であると、スパッタリング効果が大きくなり、成膜速度が低下する。以上の理由から、当該基板に対するバイアス電圧は、−１００Ｖ〜−１７０Ｖの範囲に限定した。 First, regarding the crystal structure of the hard film, the present inventor considered that it is necessary to create a local high pressure state in order to obtain a cubic structure. That is, it was considered necessary to relatively increase the energy of the film-forming substance on the substrate to be film-formed. As a method of increasing the energy, it is considered that the method of changing the bias voltage of the substrate to a negative voltage having a large absolute value is the simplest. When the voltage of the substrate exceeds a predetermined value (the absolute value is small), the energy at the time of film formation is insufficient, so that the crystal structure tends to be hexagonal. Further, when it is not more than a predetermined value (absolute value is large), the sputtering effect becomes large and the film forming speed decreases. For the above reasons, the bias voltage for the substrate was limited to the range of -100V to -170V.
次に、結晶構造が立方晶のＡｌＣｒＮ硬質皮膜は、成膜後の熱処理によって結晶構造が六方晶に変化することが試験結果から把握されている。また、基板温度が３３０℃未満であると、成膜前の脱ガス工程が不十分になり、硬質皮膜の基板に対する密着性が低下する。このことから、成膜時の基板温度は３３０℃〜３７０℃の範囲とした。 Next, it is known from the test results that the crystal structure of the AlCrN hard film having a cubic crystal structure changes to hexagonal due to the heat treatment after the film formation. Further, if the substrate temperature is less than 330 ° C., the degassing step before film formation becomes insufficient, and the adhesion of the hard film to the substrate is lowered. For this reason, the substrate temperature at the time of film formation was set in the range of 330 ° C. to 370 ° C.
なお、成膜対象がドリルやエンドミル等の切削工具である場合には、当該基板である切削工具の母材を成膜装置内に設置することができる。また、前述のターゲットのＣｒの比率が０．０５〜０．２０の範囲内である場合には、当該ターゲットを用いて成膜される硬質皮膜のＣｒ量は、０．０７〜０．２４の範囲内となる。 When the film forming target is a cutting tool such as a drill or an end mill, the base material of the cutting tool, which is the substrate, can be installed in the film forming apparatus. Further, when the ratio of Cr of the target is in the range of 0.05 to 0.20, the amount of Cr of the hard film formed by using the target is 0.07 to 0.24. It will be within the range.
本発明の実施形態について、実施例を用いて詳細に説明する。カソードアーク方式イオンプレーティング装置内に設置したステンレス製の治具上に、高速度工具鋼からなる縦６ｍｍ、横６ｍｍ、高さ４０ｍｍの直方体のブロックを基板として、６ｍｍ×４０ｍｍの面が外側に向くように固定した。この治具を毎分５回転で自転させながら、同装置に設置した電熱ヒーターにより基板温度を３７０℃として１時間加熱した。 Embodiments of the present invention will be described in detail with reference to examples. On a stainless steel jig installed in a cathode arc type ion plating device, a rectangular parallelepiped block made of high-speed tool steel with a length of 6 mm, a width of 6 mm, and a height of 40 mm is used as a substrate, and a 6 mm × 40 mm surface is on the outside. I fixed it so that it would face. While rotating this jig at 5 rpm, the substrate was heated at 370 ° C. for 1 hour by an electric heater installed in the device.
その後、基板温度を維持したまま約０．２ＰａのＡｒプラズマ中で基板をクリーニングした。このときの基板に印加したバイアス電圧は−２００Ｖとした。次に、約７Ｐａの窒素雰囲気中で各原子比率がＡｌ０．８Ｃｒ０．２の成分を持つターゲットに負の電荷を印加した状態で、電圧２４Ｖ、電流１００Ａのアーク放電を発生させた。 Then, the substrate was cleaned in Ar plasma of about 0.2 Pa while maintaining the substrate temperature. The bias voltage applied to the substrate at this time was −200 V. Next, an arc discharge with a voltage of 24 V and a current of 100 A was generated in a state where a negative charge was applied to a target having a component having an atomic ratio of Al 0.8 Cr 0.2 in a nitrogen atmosphere of about 7 Pa.
このアーク放電によりターゲットを構成する金属を蒸発させると同時にアーク放電によるイオン化を行い、反応ガス（窒素ガス）と反応させて基板上に堆積するアークイオンプレーティングを実施した。このときの基板に印加したバイアス電圧は−１５０Ｖ、基板温度を３７０℃とした。このような成膜方法による１時間の成膜で約１μｍの厚さのＡｌＣｒＮ硬質皮膜を得た。 At the same time as the metal constituting the target was evaporated by this arc discharge, ionization was performed by the arc discharge, and the arc ion plating was carried out by reacting with the reaction gas (nitrogen gas) and depositing on the substrate. The bias voltage applied to the substrate at this time was −150 V, and the substrate temperature was 370 ° C. An AlCrN hard film having a thickness of about 1 μm was obtained by forming a film for 1 hour by such a film forming method.
得られたＡｌＣｒＮ硬質皮膜は、Ｘ線回折により分析した結果、膜金属成分がＡｌ０．７６Ｃｒ０．２４であった。また、Ｘ線回折において３０°≦２θ≦９０°の範囲でＣｕ−Ｋα線の最も高い回折ピークが２θ＝３７．８°±１°であり、その半値幅は１°未満であり、硬質皮膜の結晶構造は立方晶薄膜であった。 As a result of analysis of the obtained AlCrN hard film by X-ray diffraction, the film metal component was Al 0.76 Cr 0.24 . Further, in X-ray diffraction, the highest diffraction peak of Cu−Kα rays in the range of 30 ° ≦ 2θ ≦ 90 ° is 2θ = 37.8 ° ± 1 °, and the half width is less than 1 °, which is a hard film. The crystal structure of was a cubic thin film.
実施例１と同様にイオンプレーティングによりＡｌＣｒＮ薄膜を得た。ただし、ターゲット成分はＡｌ０．８５Ｃｒ０．１５、基板に印加したバイアス電圧は−１７０Ｖ、基板の温度は３３０℃とした。得られたＡｌＣｒＮ膜は膜金属成分がＡｌ０．８３Ｃｒ０．１７であり、Ｘ線回折において、３０°≦２θ≦９０°の範囲でＣｕ−Ｋα線の最も高い回折ピークが２θ＝３７．８°±１°であり、その半値幅が１°未満の立方晶薄膜であった。 An AlCrN thin film was obtained by ion plating in the same manner as in Example 1. However, the target component was Al 0.85 Cr 0.15 , the bias voltage applied to the substrate was −170 V, and the substrate temperature was 330 ° C. The obtained AlCrN film has a film metal component of Al 0.83 Cr 0.17 , and in X-ray diffraction, the highest diffraction peak of Cu−Kα rays in the range of 30 ° ≦ 2θ ≦ 90 ° is 2θ = 37. It was a cubic thin film having a half width of 8 ° ± 1 ° and a half width of less than 1 °.
実施例１と同様にイオンプレーティングによりＡｌＣｒＮ薄膜を得た。ただし、ターゲット成分はＡｌ０．9Ｃｒ０．１、基板に印加したバイアス電圧は−１２０Ｖ、基板の温度は３５０℃とした。得られたＡｌＣｒＮ膜は膜金属成分がＡｌ０．８８Ｃｒ０．１２であり、Ｘ線回折において、３０°≦２θ≦９０°の範囲でＣｕ−Ｋα線の最も高い回折ピークが２θ＝３７．８°±１°であり、その半値幅が１°未満の立方晶薄膜であった。 An AlCrN thin film was obtained by ion plating in the same manner as in Example 1. However, the target component was Al 0.9 Cr 0.1 , the bias voltage applied to the substrate was −120 V, and the temperature of the substrate was 350 ° C. The obtained AlCrN film has a film metal component of Al 0.88 Cr 0.12 , and in X-ray diffraction, the highest diffraction peak of Cu−Kα rays in the range of 30 ° ≦ 2θ ≦ 90 ° is 2θ = 37. It was a cubic thin film having a half width of 8 ° ± 1 ° and a half width of less than 1 °.
実施例１と同様にイオンプレーティングによりＡｌＣｒＮ薄膜を得た。ただし、ターゲット成分はＡｌ０．９５Ｃｒ０．０５、基板に印加したバイアス電圧は−１５０Ｖ、基板の温度は３５０℃とした。得られたＡｌＣｒＮ膜は膜金属成分がＡｌ０．９３Ｃｒ０．０７であり、Ｘ線回折において、３０°≦２θ≦９０°の範囲でＣｕ−Ｋα線の最も高い回折ピークが２θ＝３７．８°±１°であり、その半値幅が１°未満の立方晶薄膜であった。 An AlCrN thin film was obtained by ion plating in the same manner as in Example 1. However, the target component was Al 0.95 Cr 0.05 , the bias voltage applied to the substrate was −150 V, and the temperature of the substrate was 350 ° C. The obtained AlCrN film has a film metal component of Al 0.93 Cr 0.07 , and in X-ray diffraction, the highest diffraction peak of Cu−Kα rays in the range of 30 ° ≦ 2θ ≦ 90 ° is 2θ = 37. It was a cubic thin film having a half width of 8 ° ± 1 ° and a half width of less than 1 °.
実施例１と同様にイオンプレーティングによりＡｌＣｒＴｉＮ薄膜を得た。ただし、ターゲット成分はＡｌ０．８Ｃｒ０．１５Ｔｉ０．０５、基板に印加したバイアス電圧は−１００Ｖ、基板温度は３７０℃とした。得られたＡｌＣｒＴｉＮ膜は膜金属成分がＡｌ０．７８Ｃｒ０．１７Ｔｉ０．０５であり、Ｘ線回折において３０°≦２θ≦９０°の範囲でＣｕ−Ｋα線の最も高い回折ピークは、２θ＝３７．８°±１°であり、その半値幅は１°未満の立方晶薄膜であった（本実施例５は参考例１とする）。 An AlCrTiN thin film was obtained by ion plating in the same manner as in Example 1. However, the target component was Al 0.8 Cr 0.15 Ti 0.05 , the bias voltage applied to the substrate was -100 V, and the substrate temperature was 370 ° C. The obtained AlCrTiN film has a film metal component of Al 0.78 Cr 0.17 Ti 0.05 , and the highest diffraction peak of Cu-Kα rays in the range of 30 ° ≤ 2θ ≤ 90 ° in X-ray diffraction is 2θ = 37.8 ° ± 1 °, and the half width was a cubic thin film of less than 1 ° (this Example 5 is referred to as Reference Example 1).
実施例５と同様にイオンプレーティングによりＡｌＣｒＴｉＮ薄膜を得た。ただ し、ターゲット成分はＡｌ０．８Ｃｒ０．１５Ｔｉ０．０５、基板に印加したバイアス電圧は−１２０Ｖ、基板温度は３３０℃とした。得られたＡｌＣｒＴｉＮ膜は膜金属成分がＡｌ０．７7Ｃｒ０．１8Ｔｉ０．０５であり、Ｘ線回折において３０°≦２θ≦９０°の範囲でＣｕ−Ｋα線の最も高い回折ピークは、２θ＝３７．８°±１°であり、その半値幅は１°未満の立方晶薄膜であった（本実施例６は参考例２とする）。 An AlCrTiN thin film was obtained by ion plating in the same manner as in Example 5. However, the target component was Al 0.8 Cr 0.15 Ti 0.05 , the bias voltage applied to the substrate was −120 V, and the substrate temperature was 330 ° C. The obtained AlCrTiN film has a film metal component of Al 0.77 Cr 0.18 Ti 0.05 , and the highest diffraction peak of Cu-Kα rays in the range of 30 ° ≤ 2θ ≤ 90 ° in X-ray diffraction is 2θ = 37.8 ° ± 1 °, and its half width was a cubic thin film of less than 1 ° (this Example 6 is referred to as Reference Example 2).
実施例５と同様にイオンプレーティングによりＡｌＣｒＴｉＮ薄膜を得た。ただし、ターゲット成分はＡｌ０．８Ｃｒ０．１５Ｔｉ０．０５、基板に印加したバイアス電圧は−１５０Ｖ、基板温度は３５０℃とした。得られたＡｌＣｒＴｉＮ膜は膜金属成分がＡｌ０．７６Ｃｒ０．１８Ｔｉ０．０６であり、Ｘ線回折において３０°≦２θ≦９０°の範囲でＣｕ−Ｋα線の最も高い回折ピークは、２θ＝３７．８°±１°であり、その半値幅は１°未満の立方晶薄膜であった（本実施例７は参考例３とする）。 An AlCrTiN thin film was obtained by ion plating in the same manner as in Example 5. However, the target component was Al 0.8 Cr 0.15 Ti 0.05 , the bias voltage applied to the substrate was −150 V, and the substrate temperature was 350 ° C. The obtained AlCrTiN film has a film metal component of Al 0.76 Cr 0.18 Ti 0.06 , and the highest diffraction peak of Cu-Kα rays in the range of 30 ° ≤ 2θ ≤ 90 ° in X-ray diffraction is 2θ = 37.8 ° ± 1 °, and the half width was a cubic thin film of less than 1 ° (this Example 7 is referred to as Reference Example 3).
実施例５と同様にイオンプレーティングによりＡｌＣｒＶＮ薄膜を得た。ただし、ターゲット成分はＡｌ０．８Ｃｒ０．１５Ｖ０．０５、基板に印加したバイアス電圧は−１５０Ｖ、基板温度は３５０℃とした。得られたＡｌＣｒＴｉＮ膜は膜金属成分がＡｌ０．７６Ｃｒ０．１８Ｖ０．０６であり、Ｘ線回折において３０°≦２θ≦９０°の範囲でＣｕ−Ｋα線の最も高い回折ピークは、２θ＝３７．８°±１°であり、その半値幅は１°未満の立方晶薄膜であった（本実施例８は参考例４とする）。 An AlCrVN thin film was obtained by ion plating in the same manner as in Example 5. However, the target component was Al 0.8 Cr 0.15 V 0.05 , the bias voltage applied to the substrate was −150 V, and the substrate temperature was 350 ° C. The obtained AlCrTiN film has a film metal component of Al 0.76 Cr 0.18 V 0.06 , and the highest diffraction peak of Cu-Kα rays in the range of 30 ° ≤ 2θ ≤ 90 ° in X-ray diffraction is 2θ = 37.8 ° ± 1 °, and its half width was a cubic thin film of less than 1 ° (this Example 8 is referred to as Reference Example 4).
実施例５と同様にイオンプレーティングによりＡｌＣｒＺｒＮ薄膜を得た。ただし、ターゲット成分はＡｌ０．８Ｃｒ０．１５Ｚｒ０．０５、基板に印加したバイアス電圧は−１５０Ｖ、基板温度は３５０℃とした。得られたＡｌＣｒＴｉＮ膜は膜金属成分がＡｌ０．７６Ｃｒ０．１９Ｚｒ０．０５であり、Ｘ線回折において３０°≦２θ≦９０°の範囲でＣｕ−Ｋα線の最も高い回折ピークは、２θ＝３７．８°±１°であり、その半値幅は１°未満の立方晶薄膜であった（本実施例９は参考例５とする）。 An AlCrZrN thin film was obtained by ion plating in the same manner as in Example 5. However, the target component was Al 0.8 Cr 0.15 Zr 0.05 , the bias voltage applied to the substrate was −150 V, and the substrate temperature was 350 ° C. The obtained AlCrTiN film has a film metal component of Al 0.76 Cr 0.19 Zr 0.05 , and the highest diffraction peak of Cu-Kα rays in the range of 30 ° ≤ 2θ ≤ 90 ° in X-ray diffraction is 2θ = 37.8 ° ± 1 °, and its half width was a cubic thin film of less than 1 ° (this Example 9 is referred to as Reference Example 5).
実施例５と同様にイオンプレーティングによりＡｌＣｒＮｂＮ薄膜を得た。ただし、ターゲット成分はＡｌ０．８Ｃｒ０．１５Ｎｂ０．０５、基板に印加したバイアス電圧は−１５０Ｖ、基板温度は３５０℃とした。得られたＡｌＣｒＮｂＮ膜は膜金属成分がＡｌ０．７７Ｃｒ０．１９Ｎｂ０．０４であり、Ｘ線回折において３０°≦２θ≦９０°の範囲でＣｕ−Ｋα線の最も高い回折ピークは、２θ＝３７．８°±１°であり、その半値幅は１°未満の立方晶薄膜であった（本実施例１０は参考例６とする）。 An AlCrNbN thin film was obtained by ion plating in the same manner as in Example 5. However, the target component was Al 0.8 Cr 0.15 Nb 0.05 , the bias voltage applied to the substrate was −150 V, and the substrate temperature was 350 ° C. The obtained AlCrNbN film has a film metal component of Al 0.77 Cr 0.19 Nb 0.04 , and the highest diffraction peak of Cu—Kα rays in the range of 30 ° ≦ 2θ ≦ 90 ° in X-ray diffraction is 2θ = 37.8 ° ± 1 °, and its half width was a cubic thin film of less than 1 ° (this Example 10 is referred to as Reference Example 6).
本発明の実施の形態に関する実施例は以上の通りであるが、本実施の形態とは異なる例（比較例）としての試験も行ったので、その試験条件および試験結果を以下に説明する。まず、比較例１として実施例１と同様にイオンプレーティングによりＡｌＣｒＮ薄膜を得た。ただし、ターゲット成分はＡｌ０．７Ｃｒ０．３、基板に印加したバイアス電圧は−５０Ｖ、基板温度は４５０℃とした。得られたＡｌＣｒＮ膜は膜金属成分がＡｌ０．６８Ｃｒ０．３２であり、Ｘ線回折において、３０°≦２θ≦９０°の範囲でＣｕ−Ｋα線の最も高い回折ピークが２θ＝３７．８°±１°であり、その半値幅が１°未満の立方晶薄膜であった。以上の結果より、比較例１は従来例であり、Ａｌ０．７以下であれば基板バイアスが低く、温度が高くても立方晶薄膜となることを確認した。 The examples relating to the embodiment of the present invention are as described above, but since a test as an example (comparative example) different from the embodiment of the present invention was also performed, the test conditions and test results will be described below. First, as Comparative Example 1, an AlCrN thin film was obtained by ion plating in the same manner as in Example 1. However, the target component was Al 0.7 Cr 0.3 , the bias voltage applied to the substrate was −50 V, and the substrate temperature was 450 ° C. The obtained AlCrN film has a film metal component of Al 0.68 Cr 0.32 , and in X-ray diffraction, the highest diffraction peak of Cu−Kα rays in the range of 30 ° ≦ 2θ ≦ 90 ° is 2θ = 37. It was a cubic thin film having a half width of 8 ° ± 1 ° and a half width of less than 1 °. From the above results, it was confirmed that Comparative Example 1 is a conventional example, and that if Al is 0.7 or less, the substrate bias is low, and even if the temperature is high, the cubic thin film is formed.
次に、比較例２として比較例１と同様にイオンプレーティングによりＡｌＣｒＮ薄膜を得た。ただし、ターゲット成分はＡｌ０．８Ｃｒ０．２、基板に印加したバイアス電圧は−５０Ｖ、基板温度は３５０℃とした。得られたＡｌＣｒＮ膜は膜金属成分がＡｌ０．７９Ｃｒ０．２１であったが、Ｘ線回折において、３０°≦２θ≦９０°の範囲でＣｕ−Ｋα線の最も高い回折ピークは２θ=３３°の六方晶薄膜であった。比較例１よりもＡｌ比率が高い場合、基板バイアスが低いと六方晶薄膜となることを示す例である。 Next, as Comparative Example 2, an AlCrN thin film was obtained by ion plating in the same manner as in Comparative Example 1. However, the target component was Al 0.8 Cr 0.2 , the bias voltage applied to the substrate was −50 V, and the substrate temperature was 350 ° C. The obtained AlCrN film had a film metal component of Al 0.79 Cr 0.21 , but in X-ray diffraction, the highest diffraction peak of Cu−Kα rays was 2θ = in the range of 30 ° ≦ 2θ ≦ 90 °. It was a 33 ° hexagonal thin film. This is an example showing that when the Al ratio is higher than that of Comparative Example 1, a hexagonal thin film is formed when the substrate bias is low.
次に、比較例３として比較例１と同様にイオンプレーティングによりＡｌＣｒＮ薄膜を得た。ただし、ターゲット成分はＡｌ０．８５Ｃｒ０．１５、基板に印加したバイアス電圧は−１５０Ｖ、基板温度は４５０℃とした。得られたＡｌＣｒＮ膜は膜金属成分がＡｌ０．８２Ｃｒ０．１２であったが、Ｘ線回折において、３０°≦２θ≦９０°の範囲でＣｕ−Ｋα線の最も高い回折ピークは２θ≒３３°の六方晶薄膜であった。比較例１よりもＡｌ比率が高い場合、基板温度が高いと六方晶薄膜となることを示す例である。 Next, as Comparative Example 3, an AlCrN thin film was obtained by ion plating in the same manner as in Comparative Example 1. However, the target component was Al 0.85 Cr 0.15 , the bias voltage applied to the substrate was −150 V, and the substrate temperature was 450 ° C. The obtained AlCrN film had a film metal component of Al 0.82 Cr 0.12 , but in X-ray diffraction, the highest diffraction peak of Cu−Kα rays in the range of 30 ° ≦ 2θ ≦ 90 ° was 2θ≈ It was a 33 ° hexagonal thin film. This is an example showing that when the Al ratio is higher than that of Comparative Example 1, a hexagonal thin film is formed when the substrate temperature is high.
次に、比較例４として比較例１と同様にイオンプレーティングによりＡｌＣｒＮ薄膜を得た。ただし、ターゲット成分はＡｌ０．９Ｃｒ０．１、基板に印加したバイアス電圧は−３０Ｖ、基板温度は４００℃とした。得られたＡｌＣｒＮ膜は膜金属成分がＡｌ０．８９Ｃｒ０．１１であったが、Ｘ線回折において、３０°≦２θ≦９０°の範囲でＣｕ−Ｋα線の最も高い回折ピークは２θ≒３３°の六方晶薄膜であった。比較例１よりもＡｌ比率が高い場合、基板バイアスが低く、基板温度が高いと六方晶薄膜となることを示す例である。 Next, as Comparative Example 4, an AlCrN thin film was obtained by ion plating in the same manner as in Comparative Example 1. However, the target component was Al 0.9 Cr 0.1 , the bias voltage applied to the substrate was -30 V, and the substrate temperature was 400 ° C. The obtained AlCrN film had a film metal component of Al 0.89 Cr 0.11 , but in X-ray diffraction, the highest diffraction peak of Cu−Kα rays in the range of 30 ° ≦ 2θ ≦ 90 ° was 2θ≈ It was a 33 ° hexagonal thin film. This is an example showing that when the Al ratio is higher than that of Comparative Example 1, the substrate bias is low, and when the substrate temperature is high, a hexagonal thin film is formed.
次に、比較例５として実施例４と同様にイオンプレーティングによりＡｌＣｒＮ薄膜を得た。ただし、ターゲット成分はＡｌ０．９９Ｃｒ０．０１とした。得られたＡｌＣｒＮ膜は膜金属成分がＡｌ０．９９Ｃｒ０．０１であったが、Ｘ線回折において、３０°≦２θ≦９０°の範囲でＣｕ−Ｋα線の最も高い回折ピークは２θ≒３３°の六方晶薄膜であった。実施例４よりもＡｌ比率が高いと六方晶薄膜となることを示す例である。 Next, as Comparative Example 5, an AlCrN thin film was obtained by ion plating in the same manner as in Example 4. However, the target component was Al 0.99 Cr 0.01 . The obtained AlCrN film had a film metal component of Al 0.99 Cr 0.01 , but in X-ray diffraction, the highest diffraction peak of Cu−Kα rays in the range of 30 ° ≦ 2θ ≦ 90 ° was 2θ≈ It was a 33 ° hexagonal thin film. This is an example showing that a hexagonal thin film is formed when the Al ratio is higher than that of Example 4.
次に、比較例６として実施例７と同様にイオンプレーティングによりＡｌＣｒＴｉＮ薄膜を得た。ただし、基板温度は４５０℃とした。得られたＡｌＣｒＮＴｉ膜は膜金属成分がＡｌ０．７６Ｃｒ０．１８Ｔｉ０．０６であったが、Ｘ線回折において、３０°≦２θ≦９０°の範囲でＣｕ−Ｋα線の最も高い回折ピークは２θ≒３３°の六方晶薄膜であった。実施例７で基板温度が高いと六方晶薄膜となることを示す例である。以上の本実施例１〜１０および比較例１〜６において使用したターゲットの組成、基板に印加したバイアス電圧（基板バイアス）、基板の温度（基板温度）、成膜された硬質皮膜の成分（皮膜成分）および当該硬質皮膜の結晶構造をまとめて表１に示す。 Next, as Comparative Example 6, an AlCrTiN thin film was obtained by ion plating in the same manner as in Example 7. However, the substrate temperature was 450 ° C. The obtained AlCrNTi film had a film metal component of Al 0.76 Cr 0.18 Ti 0.06 , but in X-ray diffraction, the highest diffraction of Cu-Kα rays in the range of 30 ° ≤ 2θ ≤ 90 °. The peak was a hexagonal thin film with 2θ≈33 °. In Example 7, it is an example showing that a hexagonal thin film is formed when the substrate temperature is high. The composition of the target used in Examples 1 to 10 and Comparative Examples 1 to 6 described above, the bias voltage applied to the substrate (board bias), the temperature of the substrate (board temperature), and the components of the formed hard film (film). The components) and the crystal structure of the hard film are summarized in Table 1.
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